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

HRID 62485

反応式

HRID 62485 の反応式
[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]

参加物

4

反応物 2

HCID 6329MethylamineHCID 2885605-Fluoroisatoic anhydride

生成物 1

HCID 431325582-Amino-5-fluoro-N-methylbenzamide収率 65%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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)+

後処理

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

出典と根拠

ORDレコード
ord-aef9e4fc5a7a44e5a961eff5a775f7f9
出典データセット
uspto-grants-2016_09
特許番号
US09446034B2

関連ノート

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