2-Chloroethanol → 4-Hydroxy-2'-nitrobutyrophenone

HRID 1198755ノート

反応式

HRID 1198755 の反応式
[N+:1]([C:4]1[CH:17]=[CH:16][CH:15]=[CH:14][C:5]=1[C:6]([CH2:8][C:9](OCC)=O)=[O:7])([O-:3])=[O:2].ClC[CH2:20][OH:21].[OH-].[Na+].[OH-].C([N+](C)(C)C)C1C=CC=CC=1>O>[OH:21][CH2:20][CH2:9][CH2:8][C:6]([C:5]1[CH:14]=[CH:15][CH:16]=[CH:17][C:4]=1[N+:1]([O-:3])=[O:2])=[O:7]

参加物

6

反応物 4

HCID 342-ChloroethanolHCID 14798Sodium HydroxideHCID 66854Benzyltrimethylammonium hydroxideHCID 10561837Ethyl 2-nitro-beta-oxobenzenepropanoate

生成物 1

HCID 109767084-Hydroxy-2'-nitrobutyrophenone

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of ethyl 2-(o-nitrobenzoyl)acetate (11.9 g, 0.05 mol), 2-chloroethanol (8 g, 0.1 mol), 50% sodium hydroxide solution (8.8 g, 4.4 g real, 0.11 mol) and 40% benzyltrimethylammonium hydroxide solution (4.2 PG,12 g, 1.7 g, real, 0.01 mol) in water (50 mL) is heated at 50°-65° C. for 4-8 hours, cooled and extracted with methylene chloride. The combined organic extracts are concentrated in vacuo to give the title product, identified by 1HNMR and 13CNMR analyses.

後処理

  1. temperatureis heated at 50°-65° C. for 4-8 hours
  2. temperaturecooled
  3. extractionextracted with methylene chloride
  4. concentrationThe combined organic extracts are concentrated in vacuo

出典と根拠

ORDレコード
ord-f67cba12d1774568ba0a99d4ef24dae6
出典データセット
uspto-grants-1994_01
特許番号
US05281726

反応ノート

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