Hydrochloric Acid → HCID 584994、化合物

HRID 398016ノート

反応式

HRID 398016 の反応式
[CH3:1][O:2][C:3]1[CH:11]=[CH:10][CH:9]=[CH:8][C:4]=1[C:5](Cl)=[O:6].[OH:12][CH2:13][C:14]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)=[O:15].Cl>N1C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:11]=[CH:10][CH:9]=[CH:8][C:4]=1[C:5]([O:12][CH2:13][C:14]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)=[O:15])=[O:6]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 68490alpha-HydroxyacetophenoneHCID 889692-Methoxybenzoyl chloride

生成物 1

HCID 584994HCID 584994、化合物収率 89.6%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
60 °C

実験手順

2-Methoxybenzoyl chloride (about 51 g) from Example 1a was added dropwise to a mixture of 2-hydroxyacetophenone (27.2 g, 24.1 ml, 0.20 mol) and pyridine (40 ml). The reaction mixture was warmed to about 60° C. exothermically. After stirring for 15 minutes, the reaction mixture was poured onto a mixture of ice (800 g) and 36% hydrochloric acid (120 ml). The solid was filtered off, washed with water, and dried. The crude product was crystallized from methanol to yield 48.4 g (89.6%) of the compound (m.p.: 78-79° C.).

後処理

  1. filtrationThe solid was filtered off
  2. washwashed with water
  3. customdried
  4. customThe crude product was crystallized from methanol

出典と根拠

ORDレコード
ord-a19d9f6c87f2437ca159bf0317799e60
出典データセット
uspto-grants-2003_08
特許番号
US06610738B2

反応ノート

読み込み中…