7. RESULTADOS
7.3 BARRERAS PARA LA IMPLEMENTACIÓN DE ACCIONES INTERSECTORIALES
7.3.5 Dificultades en la respuesta comunitaria
se p arate d a t once from th e g re e i so lu tio n* These T?©ve oollG C ied, vraahed w ith a o e tio a c id, and on ic in g suspended In w ater ( 2 5 m l.), Im m ediately beoame blue# A fter b ein g
shaken fo r JO m inutes, to com plete h y d ro ly sis, th e blue
s o lid was f il tv r e d o f l, washed w ith w ater u n t i l fre e o f a o id, and d rie d in vnouo. l-iW )im ethiilam inob#isylidonm sulcaium
p e rc h lo ra te was thus obtained as c r y a ta ls which m elt
to a b lu e ta r on a b lo ck p reh eated to <|C 2 1 0®.
Found; 0 6 6 . 4 H 5 . 4 N 4 .7 ,
Ci^Hi8C1H04 re q u ire s 6 j # 4 5 # 0 J.gf^
X max. ( a o e to n itr ile ) 655.
CI 2J AsuXene w jth 2-F u r1uraldchyde
Azulene (1 ) 2 Ru?a. ), 2-lu riu rn ld e h ;/d e ( 1 4 4 mya.) and
a c ctio acid ( 8 m l.) w ith p e rc h lo ric ao id (0 .5 m l.) gave a
b rig h t red o o lu tlo n . - u ry lld m e^ m lm iu m perchlogQ.te
(415 m/TS., 901^') c r y s ta llis e d ne orange n e e d le s, and, a ft e r being waohed w ith a o o tio aoid follow ed by muoh e th e r, i t was d rie d lo r 2 0 m inutes a t 1 1 0®. M.p. 1 7 9®"l8l® (b lo ck
p reh eated to 175®)#
^Pund; G 56.1 R J .9 01 1 2. 4 ,
- 159 “
X max* ( a o eto n itr ile ) 4 )6 .
CI 2 4 AAulene w ith V P ew iy lln ao le
A m ixture o f azulone ( 1 2 8 ) and 3-io rm y lln d o le
(145 m ge.) in ao«^tlo n cid (10 n l* ), tre a te d w ith p ro h lo rle a cid (0 .5 m l.), y ie ld e d l - 3 '-iadolylm ethyleneam uleniem
p c rg h lo m te (305 mga., 89K) as v io lew b la c ii n eed les which were waohed w ith a c e tic meld follow ed by e th e r, and d rie d fo r 20 m inutes a t 110®# The iro d u o t m elts to a v io le t liq u id on a block p reh eated to 2/0®, b ut decomposes
slow ly to a b la c k ta r on being honied from room tem perature* Found; H J#6 Cl 9 .6 ,
Cj^gHj^l^ClHOi^ re q u ire s 4 . 1 1 0#J f
X max. ( a o e to n itr ile ) 560.
01 25 4 ^6»8-T riaethyX ajm lcnej^L ith 2-1 u riu rald eh y d e
A s o lutio n ox 4 ,6 ,8 —trim c th y la su lo n e (168 mgn.) and 2-fu rfu rald eh y d o (100 m gs.) in a o etio acid
(8
m l.) imstre a te d w ith p e rc h lo ric aoid (0 .5 m l.), at room teirg;>ernture. The m ixture turned bro\m, and c r y sta l lis a t io n be^ian a t
once# A lter 1 0 m inuter,, lig ht rown n eed les o f l - (2-lu ry lV
m eth y le n ^4 .6 .8-trlia e t.h y la » u lc n lu a p cv g h lo rate (35 m.;8.,
10?) were f il te r e d 01f, w nhed i t h e th e r and d rie d in vacuo. H c c ry a ta llie a tio n W'.e from nee t i e a c id . The p ro d u ct deotmqioeed w ithout m elting above 200®.
Found} C 62,0 IÎ 4 .9 Cl 1 0. 2,
- i6o -
CI 26 O oalnaulene w ith A oatalcchgde
The o rd er o f mixing of the rc n o ta n ts Is o r l t l o n l, and
th e follow ing lo th e moot a a tlo fo e to ry procedure.
P e rc h lo ric acid (0 , 5 m l.) wna added to a s o lu tio n o f
gualnzulcnc (200 mga.) and acctaldehydo (1,5 m l.) In et r a-
hydrofuran ( 1 m l.) at room to n p c ra tu re . 0-Sth.vlldeaem jnl-
aaulcnluri p e rc h lo rate (310 a s ., 96f) c r y ata llie e d a ttc p
1—2 m inutes, as i Ine yellow n e e d le s. Theee were tv ached w ith te tra h y d ro fu ra n fo llo w id by e th e r and d rie d In vacuo, M.p. 161-165 . The s a lt decoriposes In hot so lv e n ts and was
analysed w ithout r e c r y s ta llls n tlo n a f t . r d ry in g f o r 8 hours a t 70®/0«1 m.m.
round} 0 62.1 H 6 .1 01 11.2,
Gj^-Hg^ClOji^ requlrcD 62.9 6 .5 1 0 .9 ?
\ max. ( a c e tic a c id ) 425 (sh o u ld e r) ( 3.4 5 ) , 3 7 0 (3 .7 5 ).
CI 27 4.^6.8-T rim eth y lazu len e w ith ioetaldebvda
A s o lu tio n o i 4 , 6 ,8-trlm e th y la z u le n e (763 mge.) and
aoetaldehydo (3 m l.) in a c e tic mold (10 m l.) was tre a te d w ith p e rc h lo ric a d d (1 m l.). l- K th y lld e n e- h .6 .8 -tr l
m
th v l-aaulonlum p e rc h lo rate (II7 0 im e ., 8fi?) o ry atm llieo d ma
g ro e n la h-y e llo^ ne d le a, which wer, washed w ith a o r tic a cid follow ed by e th e r, and d rie d in vnouo. M.p. 148-15 1° ( d ) ,
This was analysed w ithout r e o r y e tn ilis n tio n . vound} C 60,7 n 6. 0 ,
— l 6l —
\ max. (n o e to n itp llo ) 405 (broad) (3 .6 6 ), \ wax. (n o e tic a c id ) 44O (shoulcier) (3 .5 0 ).
X max. (no t i c acid conta in i 2, (v /v ) p e rc h lo ric a c id )
395 (broad) (3 .7 0 ).
CI 28 aw aU guiene w ith Oinnamalctohrde
(Kiaiazulcnio (2(X) mga# ) and cinnaoaldch.'/’ o (132 m ?s.), d leao lv cd in to tra h y d ro lu rn n (2 m l.), and tr e a te d w ith p e r c h lo ric a c id (0,5 m l.) at room tem p ératu re, y ie ld ed
3-olnnagylldenem iainaulenlum p e rc h lo rate (212 ki 'b ., 50?) as
d ark red neodleo. A fte r re c ry B tn llia n tio n Iro n aoi t i c a c id,
th e m.p. m s 2l8«224®(d).
round; C 70.3 H 5.9 0 1 8 .1,
02i,H25ClOj^ ponuires 69.8 6,1 8 .6 ? Xmnx. ( a c etic n c id ) 515 (4 .6 3 ).
CI 29 C uaingulene w ith Phoni'/laoctaldeh/de
Phonylaoetaldehycie ( 2 0 0 m a .) wno added to a m lxture o f
guaiaaulene (200 mga. ), te tra h y d ro iu m n (1 m l.) and p e rc h lo ric a c id (0 .5 m l.). A yoilow lsh-Trown sem l-o ry st a l l i n e s o lid
(85 rafi®*)» w ith m.p. 92-98®, was i i l t o r e d o f f, washed w ith te tra h y d ro fu ra n and d rie d in vacuo. Thla p ro d u ct, however, could n ot bo p u r if ie d . The ab so rp tio n spectrum (n o e tic a o id ) showed no maxioain in th e v is ib l e region, only o p ro g re ssiv e slo p e upwards in to the
u.v.
re g io n .Numerous v a r ia tio n s to th e exjn rim ent procedure w ith re sp e c t to the p ro p o rtio n s of components and o rcer o f mixing were tr ie d w ithout su c c e ss. N othing could be is o la te d a f t e r
— i 62 —