6-methoxy-2,4-dihydro-1H-3,1-benzoxazine-2,4-dione → 4-(2,4-Dimethoxy-benzyl)-7-methoxy-3,4-dihydro-1H-benzo[e][1,4]diazepine-2,5-dione

HRID 351827

反応式

HRID 351827 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[NH:11][C:10](=[O:12])O[C:8](=[O:13])[C:7]=2[CH:14]=1.[CH3:15][O:16][C:17]1[CH:28]=[C:27]([O:29][CH3:30])[CH:26]=[CH:25][C:18]=1[CH2:19][NH:20][CH2:21]C(O)=O>CC1C=CC(C)=CC=1>[CH3:15][O:16][C:17]1[CH:28]=[C:27]([O:29][CH3:30])[CH:26]=[CH:25][C:18]=1[CH2:19][N:20]1[C:8](=[O:13])[C:7]2[CH:14]=[C:3]([O:2][CH3:1])[CH:4]=[CH:5][C:6]=2[NH:11][C:10](=[O:12])[CH2:21]1

参加物

4

反応条件

温度
140 °C

実験手順

6-Methoxy-2H-3,1-benzoxazine-2,4(1H)-dione (23 g, 119 mmol) and (2,4-dimethoxy-benzylamino)-acetic acid 1 (27 g, 120 mmol) were suspended in p-xylene (500 mL) and heated under argon at reflux (140° C.) for 2 h. The hot solution was allowed to cool to rt, while spontaneous crystallization occurred. The crystals were filtered off and washed with p-xylene (50 mL). Yield: 39 g (92%). mp 196° C. m/z 356 (M).

後処理

  1. temperatureheated under argon
  2. temperatureto cool to rt, while spontaneous crystallization
  3. filtrationThe crystals were filtered off
  4. washwashed with p-xylene (50 mL)

出典と根拠

ORDレコード
ord-1bdefbd3eca540f7b727c2ddaf516e60
出典データセット
uspto-grants-2004_06
特許番号
US06743789B2

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