Hydrochloric Acid → HCID 178444277, 화합물

HRID 247529노트

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HRID 247529 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([O:11][C:12]([C:14]2[CH:19]=[CH:18][C:17]([C:20]3[CH:25]=[CH:24][C:23]([C@H:26]4[CH2:31][CH2:30][C@H:29]([CH2:32][CH2:33][CH2:34][CH2:35][CH3:36])[CH2:28][CH2:27]4)=[CH:22][CH:21]=3)=[CH:16][CH:15]=2)=[O:13])[CH:5]=[CH:6][C:7]=1[C:8](Cl)=[O:9].[Cl:37][C:38]1[CH:39]=[C:40]([OH:47])[CH:41]=[CH:42][C:43]=1[N+:44]([O-:46])=[O:45].Cl>C1C=CC=CC=1.N1C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[C:4]([O:11][C:12]([C:14]2[CH:19]=[CH:18][C:17]([C:20]3[CH:21]=[CH:22][C:23]([C@H:26]4[CH2:31][CH2:30][C@H:29]([CH2:32][CH2:33][CH2:34][CH2:35][CH3:36])[CH2:28][CH2:27]4)=[CH:24][CH:25]=3)=[CH:16][CH:15]=2)=[O:13])[CH:5]=[CH:6][C:7]=1[C:8]([O:47][C:40]1[CH:41]=[CH:42][C:43]([N+:44]([O-:46])=[O:45])=[C:38]([Cl:37])[CH:39]=1)=[O:9]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 102833-Chloro-4-nitrophenolHCID 178444276HCID 178444276, 화합물

생성물 1

HCID 178444277HCID 178444277, 화합물

시약·촉매·용매 2

HCID 241Benzene용매HCID 1049Pyridine용매

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온도
65 °C

실험 절차

The crude 4'-(trans-4-pentylcyclohexyl)-4-biphenylcarboxylic acid 3-chloro-4-(chlorocarbonyl)phenyl ester obtained was dissolved in 150 ml of benzene and then added dropwise to a solution of 1.2 g of 3-chloro-4-nitrophenol in 110 ml of dry pyridine. The mixture was stirred at 65° C. overnight, then poured into a mixture of 500 ml of ice-water and 100 ml of concentrated hydrochloric acid and extracted with diethyl ether. The extract was washed three times with 100 ml of 3N hydrochloric acid each time and three times with 200 ml of water each time, then dried and evaporated. The crude 4'-(trans-4-pentylcyclohexyl)-4-biphenylcarboxylic acid 3-chloro-4-[(3-chloro-4-nitrophenoxy)carbonyl]phenyl ester obtained was chromatographed on silica gel with toluene/acetone (volume ratio 19:1). The fractions which were almost pure according to thin-layer chromatography (2.8 g) were recrystallized twice from ethyl acetate; m.p. (C-N) 132° C., cl.p. >250° C. (decomposition).

후처리

  1. extractionextracted with diethyl ether
  2. washThe extract was washed three times with 100 ml of 3N hydrochloric acid each time and three times with 200 ml of water each time
  3. customdried
  4. customevaporated

출처 및 근거

ORD 기록
ord-2681b2e555344b4f95857442aee4ed08
출처 데이터셋
uspto-grants-1987_11
특허 번호
US04708441

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