Methylamine → cis N-methyl-4-(2-fluoro-5-bromobenzyloxy)but-2-enylamine

HRID 1066855노트

반응식

HRID 1066855 반응식
[F:1][C:2]1[CH:14]=[CH:13][C:12]([Br:15])=[CH:11][C:3]=1[CH2:4][O:5][CH2:6][CH:7]=[CH:8][CH2:9]Br.[CH3:16][NH2:17]>O1CCCC1>[CH3:16][NH:17][CH2:9]/[CH:8]=[CH:7]\[CH2:6][O:5][CH2:4][C:3]1[CH:11]=[C:12]([Br:15])[CH:13]=[CH:14][C:2]=1[F:1]

참가 물질

4

반응물 2

HCID 6329MethylamineHCID 539384814-(2-Fluoro-5-bromobenzyloxy)but-2-enyl bromide

생성물 1

HCID 59958653cis N-methyl-4-(2-fluoro-5-bromobenzyloxy)but-2-enylamine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

In a 250 ml flask 4-(2-fluoro-5-bromobenzyloxy)but-2-enyl bromide (1.968 g, 5.89 mmol) was dissolved in dry tetrahydrofuran (40 5 ml). To this solution methylamine (29.5 ml, 58.9 mmol) was added in one portion and the resulting mixture was stirred at ambient temperature for five hours. The progress of the reaciton was monitored by thin layer chromatography. The solvents were removed in vacuo and the residue was taken up in 1 M potassium carbonate and extracted thrice 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 liquid chromatography.

후처리

  1. customThe solvents were removed in vacuo
  2. extractionextracted thrice 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 liquid chromatography

출처 및 근거

ORD 기록
ord-730a0feaaad94f4e99d6c72420dead5f
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06245761B1

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