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

HRID 2059016

反応式

HRID 2059016 の反応式
[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

参加物

5

反応物 4

HCID 962Water4 回HCID 1049PyridineHCID 8396o-CyclohexylphenolHCID 884383-Pyridinecarbonyl chloride, hydrochloride (1:1)

生成物 1

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

実験手順

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 was obtained from the filtrate by further adding water (60 ml).

後処理

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

出典と根拠

ORDレコード
ord-edcbb938a5cc4981bed4d3f83df746ef
出典データセット
uspto-grants-1982_03
特許番号
US04321268

関連ノート

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