Water → HCID 178444240, 화합물

HRID 1421198노트

반응식

HRID 1421198 반응식
[C:1](=S)=S.[CH2:4]([C@H:9]1[CH2:14][CH2:13][C@H:12]([C:15]2[CH:20]=[CH:19][C:18]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)=[CH:17][CH:16]=2)[CH2:11][CH2:10]1)[CH2:5][CH2:6][CH2:7][CH3:8].[Cl-].[Al+3].[Cl-].[Cl-].[CH:31]1(C(Cl)=O)[CH2:36][CH2:35][CH2:34][CH2:33][CH2:32]1.[OH2:40]>>[CH2:4]([C@H:9]1[CH2:14][CH2:13][C@H:12]([C:15]2([C:31]3[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=3)[CH:16]=[CH:17][C:18]([CH:21]3[CH2:22][CH2:23][CH2:24][CH2:25][CH2:26]3)=[CH:19][C:20]2=[C:1]=[O:40])[CH2:11][CH2:10]1)[CH2:5][CH2:6][CH2:7][CH3:8]

참가 물질

6

반응물 5

HCID 962Water2회HCID 6348Carbon DisulfideHCID 75938Cyclohexanecarbonyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 178444253HCID 178444253, 화합물

생성물 1

HCID 178444240HCID 178444240, 화합물

실험 절차

First, 127 parts of carbon disulfide, 15.3 parts of 4-(trans-4-pentylcyclohexyl)biphenyl (produced by Kanto Kagaku Kabushiki Kaisha), and 8.4 parts of anhydrous aluminum chloride are mixed together. While cooling the mixture with iced water, 8.1 parts of cyclohexane carbonyl chloride is dropped to the mixture at 5° C. or less. After the resultant mixture is stirred at 5° C. or less for 2 hours and then at 15° C. to 20° C. for another 2 hours, the reaction mixture is put into 100 parts of iced water and decomposed. Then, the carbon disulfide layer is separated and washed with water 3 times. Then, carbon disulfide is distilled off. Thus, crude 1-(trans-4-pentylcyclohexyl)-4-cyclohexyl carbonyl biphenyl is obtained.

후처리

  1. additionis dropped to the mixture at 5° C. or less
  2. customThen, the carbon disulfide layer is separated
  3. washwashed with water 3 times
  4. distillationThen, carbon disulfide is distilled off

출처 및 근거

ORD 기록
ord-8f4419a2ef3a436ab32af29cd210b88b
출처 데이터셋
uspto-grants-2000_06
특허 번호
US06074708

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