Ethyl chloroacetate → HCID 18623221、化合物

HRID 324309ノート

反応式

HRID 324309 の反応式
[H-].[Na+].[NH2:3][CH:4]([C:7]1[CH:12]=[CH:11][C:10]([F:13])=[C:9]([F:14])[CH:8]=1)[CH2:5][OH:6].Cl[CH2:16][C:17](OCC)=[O:18]>C1COCC1>[F:14][C:9]1[CH:8]=[C:7]([CH:4]2[NH:3][C:17](=[O:18])[CH2:16][O:6][CH2:5]2)[CH:12]=[CH:11][C:10]=1[F:13]

参加物

5

反応物 3

HCID 7751Ethyl chloroacetateHCID 24758Sodium hydrideHCID 220488782-Amino-2-(3,4-difluorophenyl)ethanol

生成物 1

HCID 18623221HCID 18623221、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

To a suspension of NaH (8.0 mmol, 0.19 g) in 10 mL THF at 0° C. was added a solution of 2-amino-2-(3,4-difluorophenyl)-ethanol (7.51 mmol, 1.3 g) in 20 mL THF dropwise via an addition funnel and after 30 min ethyl chloroacetate was added dropwise via syringe. The orange colored reaction mixture was stirred for 2 hours at 0° C. and then for 2 hours at 35° C. The solvent was removed and the 5-(3,4-difluoro-phenyl)-morpholin-3-one was isolated as a thick yellow oil (0.5 g). 1H NMR showed that the product was about 85% pure and any attempts to purify it further by column chromatography were not successful. It was used in the next reaction as described below without further purification.

後処理

  1. waitfor 2 hours at 35° C
  2. customThe solvent was removed

出典と根拠

ORDレコード
ord-cfad788125bb4e4dbc8277df133493c4
出典データセット
uspto-grants-2001_04
特許番号
US06218390B1

反応ノート

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