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

HRID 1198755노트

반응식

HRID 1198755 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 109767084-Hydroxy-2'-nitrobutyrophenone

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f67cba12d1774568ba0a99d4ef24dae6
출처 데이터셋
uspto-grants-1994_01
특허 번호
US05281726

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