Diethylamine → N,N-dimethyl-4-(2-fluoro-5-bromobenzyloxy)butylamine

HRID 1066830ノート

反応式

HRID 1066830 の反応式
[CH2:1]([NH:3][CH2:4]C)C.[F:6][C:7]1[CH:19]=[CH:18][C:17]([Br:20])=[CH:16][C:8]=1[CH2:9][O:10][CH2:11][CH2:12][CH2:13][CH2:14]Br>O1CCCC1.C(Cl)Cl>[CH3:1][N:3]([CH2:14][CH2:13][CH2:12][CH2:11][O:10][CH2:9][C:8]1[CH:16]=[C:17]([Br:20])[CH:18]=[CH:19][C:7]=1[F:6])[CH3:4]

参加物

5

反応物 2

HCID 8021DiethylamineHCID 21196139HCID 21196139、化合物

生成物 1

HCID 21196124N,N-dimethyl-4-(2-fluoro-5-bromobenzyloxy)butylamine

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Diethylamine (17.6 ml, 35.3 mmol) was added to a solution of 4-(2-fluoro-5-bromobenzyloxy)butyl bromide (1.2 g, 3.53 mmol) in tetrahydrofuran (18 ml). The resulting mixture was stirred at ambient temperature for about 18 hours. The reaction mixture was diluted with methylene chloride and washed with saturated sodium bicarbonate. The aqueous fraction was back extracted with methylene chloride. The organic fractions were combined and dried over sodium sulfate. The solvents were removed in vacuo. The desired title intermediate was further purified by high performance liquid chromatography.

後処理

  1. washwashed with saturated sodium bicarbonate
  2. extractionThe aqueous fraction was back extracted with methylene chloride
  3. dry with materialdried over sodium sulfate
  4. customThe solvents were removed in vacuo
  5. customThe desired title intermediate was further purified by high performance liquid chromatography

出典と根拠

ORDレコード
ord-ffa301ccf12f48d99f0b6e2c31eb9711
出典データセット
uspto-grants-2001_06
特許番号
US06245761B1

反応ノート

読み込み中…