Hydrochloric Acid → 3-Cyano-4-(2'-methylbutyl)benzoic acid 4'-octyloxy-4-biphenylyl ester

HRID 2072609노트

반응식

HRID 2072609 반응식
[CH2:1]([O:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]2[CH:21]=[CH:20][C:19]([O:22][C:23](=[O:36])[C:24]3[CH:29]=[CH:28][C:27]([CH2:30][CH:31]([CH3:34])[CH2:32][CH3:33])=[C:26](Br)[CH:25]=3)=[CH:18][CH:17]=2)=[CH:12][CH:11]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].[CH3:37][N:38](C)C=O.Cl.O>C1(C)C=CC=CC=1>[CH2:1]([O:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]2[CH:21]=[CH:20][C:19]([O:22][C:23](=[O:36])[C:24]3[CH:29]=[CH:28][C:27]([CH2:30][CH:31]([CH3:34])[CH2:32][CH3:33])=[C:26]([C:37]#[N:38])[CH:25]=3)=[CH:18][CH:17]=2)=[CH:12][CH:11]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 6228DimethylformamideHCID 542993093-Bromo-4-(2'-methylbutyl)benzoic acid 4'-octyloxy-4-biphenylyl ester

생성물 1

HCID 147668273-Cyano-4-(2'-methylbutyl)benzoic acid 4'-octyloxy-4-biphenylyl ester

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of this 3-bromo-4-(2'-methylbutyl)benzoic acid 4-octyloxy-4'-biphenylyl ester (5.5 g, 0.01 mol), cuprous cyanide (1.1 g, 0.06 mol) and dimethylformamide (20 ml) was heated to 145°-147° C., following by agitating it for 6 hours, adding a mixture of ferric chloride (4 g), hydrochloric acid (1 ml) and water (7 ml), keeping the mixture at 60°-70° C. for 15 minutes, feeding it into ice water, adding toluene, sufficiently agitating the mixture, transferring it into a separating funnel, several times washing the resulting organic layer with water, drying it over anhydrous MgSO4, distilling off toluene and recrystallizing the residue from ethanol (50 ml) to obtain the objective 3-cyano-4-(2'-methylbutyl)benzoic acid 4'-octyloxy-4-biphenylyl ester (1.7 g). The phase transition points of this product were as follows: ##STR46##

후처리

  1. temperaturewas heated to 145°-147° C.
  2. additionadding
  3. customat 60°-70° C.
  4. customfor 15 minutes
  5. stirringsufficiently agitating the mixture
  6. washseveral times washing the resulting organic layer with water
  7. dry with materialdrying it over anhydrous MgSO4
  8. distillationdistilling off toluene
  9. customrecrystallizing the residue from ethanol (50 ml)

출처 및 근거

ORD 기록
ord-96cb0a630d2a4f9497fedc2c137a7e7d
출처 데이터셋
uspto-grants-1990_04
특허 번호
US04913838

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