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

HRID 1066830노트

반응식

HRID 1066830 반응식
[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]

참가 물질

5

반응물 2

HCID 8021DiethylamineHCID 21196139HCID 21196139, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ffa301ccf12f48d99f0b6e2c31eb9711
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06245761B1

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