Dichloromethane → HCID 19871100、化合物

HRID 329595

反応式

HRID 329595 の反応式
C(O)(=O)C(O)=O.[CH:7]([NH:10][OH:11])([CH3:9])[CH3:8].[OH-].[Na+].[Br:14][CH:15]([CH2:19]Br)[C:16](Cl)=[O:17].C(Cl)Cl>O>[Br:14][CH:15]1[CH2:19][O:11][N:10]([CH:7]([CH3:9])[CH3:8])[C:16]1=[O:17]

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 14798Sodium Hydroxide3 回HCID 867902,3-Dibromopropanoyl chlorideHCID 19871111HCID 19871111、化合物

生成物 1

HCID 19871100HCID 19871100、化合物収率 63.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

To a stirred mixture of 6 g (25 mmol) of N-isopropylhydroxylamine oxalate and 1N sodium hydroxide (50 ml) in water (100 ml) cooled to 0° C. there was added 2,3-dibromopropionyl chloride (12.5 g, 50 mmol), followed by the addition of 50 ml of 1N sodium hydroxide. Ten minutes later, 150 ml of methylene chloride and 60 ml of 1N sodium hydroxide were added. The mixture was stirred continuously for one hours following which the organic phase was separated, dried over anhydrous magnesium sulfate and concentrated. The concentrate was chromatographed on silica gel with 40% ethyl acetatehexane to afford 3.3 g of 4-bromo-2-isopropyl-3-isoxazolidinone.

後処理

  1. customwas separated
  2. dry with materialdried over anhydrous magnesium sulfate
  3. concentrationconcentrated
  4. customThe concentrate was chromatographed on silica gel with 40% ethyl acetatehexane

出典と根拠

ORDレコード
ord-730eb489b9ec4f098361805efb92dc25
出典データセット
uspto-grants-1990_01
特許番号
US04892870

関連ノート

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