Methylamine → 2-Amino-5-fluoro-N-methylbenzamide

HRID 62485

반응식

HRID 62485 반응식
[F:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:10]C(=O)[O:8][C:7](=O)[C:6]=2[CH:13]=1.[CH3:14][NH2:15]>O1CCCC1>[NH2:10][C:5]1[CH:4]=[CH:3][C:2]([F:1])=[CH:13][C:6]=1[C:7]([NH:15][CH3:14])=[O:8]

참가 물질

4

반응물 2

HCID 6329MethylamineHCID 2885605-Fluoroisatoic anhydride

생성물 1

HCID 431325582-Amino-5-fluoro-N-methylbenzamide수율 65%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

6-Fluoro-2H-3,1-benzoxazine-2,4(1H)-dione (200 mg, 1.104 mmol) was dissolved in dry tetrahydrofuran (THF) (10 mL), at which time methyl amine (3.31 mL, 6.63 mmol) was added. The reaction was stirred at room temperature for 1 h, then concentrated under vacuum. The crude product was purified on silica (Biotage, 40% EtOAc/hexene) to afford the title compound (120 mg, 65%) as a white solid. LC-MS (ES) m/z=169.1 (M+H)+

후처리

  1. additionwas added
  2. concentrationconcentrated under vacuum
  3. customThe crude product was purified on silica (Biotage, 40% EtOAc/hexene)

출처 및 근거

ORD 기록
ord-aef9e4fc5a7a44e5a961eff5a775f7f9
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09446034B2

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