Water → Nicotinic acid, p-cyclohexylphenyl ester (7CI,8CI)

HRID 1648741

반응식

HRID 1648741 반응식
[CH:1]1([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2O)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.Cl.[C:15](Cl)(=[O:22])[C:16]1[CH:21]=[CH:20][CH:19]=[N:18][CH:17]=1.N1C=CC=CC=1.[OH2:30]>>[C:15]([O:22][C:10]1[CH:11]=[CH:12][C:7]([CH:1]2[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]2)=[CH:8][CH:9]=1)(=[O:30])[C:16]1[CH:21]=[CH:20][CH:19]=[N:18][CH:17]=1

참가 물질

5

반응물 4

HCID 962Water4회HCID 1049PyridineHCID 8396o-CyclohexylphenolHCID 884383-Pyridinecarbonyl chloride, hydrochloride (1:1)

생성물 1

HCID 198853Nicotinic acid, p-cyclohexylphenyl ester (7CI,8CI)

실험 절차

17.6 g (100 mmol) of cyclohexylphenol and 19 g (106 mmol) of nicotinic acid chloride hydrochloride was mixed with 250 ml of dry pyridine and kept at 40° C. for 4 hours. Subsequently, the mixture was cooled in the ice bath, and water added in portions. After addition of 10 ml of water a clear solution was obtained. Water (50 ml) was admixed until strong turbidity appeared. After stirring the mixture for a longer period of time the product crystallized in the ice bath. The precipitate was sucked off, freed from pyridine by washing with water and dried. A second fraction as obtained from the filtrate by further adding water (60 ml).

후처리

  1. additionadded in portions
  2. customwas obtained
  3. customcrystallized in the ice bath
  4. washby washing with water
  5. customdried
  6. customA second fraction as obtained from the filtrate

출처 및 근거

ORD 기록
ord-c939a5c66da24794a03bff3fa3a49a52
출처 데이터셋
uspto-grants-1983_11
특허 번호
US04412998

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