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Methylamine → N-Methyl-2-{4-[(3-oxo-3,4-dihydro-2H-1,4-benzoxazin-6-yl)carbonyl]-3,4-dihydro-2H-1,4-benzoxazin-3-yl}acetamide

HRID 1054181
ノート
印刷プレビュー

反応式

HRID 1054181 の反応式
[CH3:1][NH2:2].[O:3]=[C:4]1[NH:9][C:8]2[CH:10]=[C:11]([C:14]([N:16]3[C:21]4[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=4[O:19][CH2:18][CH:17]3[CH2:26][C:27](OCC)=[O:28])=[O:15])[CH:12]=[CH:13][C:7]=2[O:6][CH2:5]1>CO>[CH3:1][NH:2][C:27](=[O:28])[CH2:26][CH:17]1[N:16]([C:14]([C:11]2[CH:12]=[CH:13][C:7]3[O:6][CH2:5][C:4](=[O:3])[NH:9][C:8]=3[CH:10]=2)=[O:15])[C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=2[O:19][CH2:18]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6329MethylamineHCID 131736322Ethyl {4-[(3-oxo-3,4-dihydro-2H-1,4-benzoxazin-6-yl)carbonyl]-3,4-dihydro-2H-1,4-benzoxazin-3-yl}acetate2 回

生成物 1

HCID 118599697N-Methyl-2-{4-[(3-oxo-3,4-dihydro-2H-1,4-benzoxazin-6-yl)carbonyl]-3,4-dihydro-2H-1,4-benzoxazin-3-yl}acetamide収率 100%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Methylamine (370 mL) was added slowly into a solution of ethyl {4-[(3-oxo-3,4-dihydro-2H-1,4-benzoxazin-6-yl)carbonyl]-3,4-dihydro-2H-1,4-benzoxazin-3-yl}acetate (Intermediate 4, 10.7 g, 26.9 mmol) in MeOH (640 mL) at rt. The resulting mixture was stirred at rt for 16 h. The organic solvent was removed by evaporation under reduced pressure. The crude product was purified by re-crystallization from MeOH to afford the title compound (10.3 g, 100%) as a white power.

後処理

  1. customThe organic solvent was removed by evaporation under reduced pressure
  2. customThe crude product was purified by re-crystallization from MeOH

出典と根拠

ORDレコード
ord-02d035f75f474f74ad7fd1d305db702d
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09394291B2

反応ノート

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