5-Bromoisatoic Anhydride → 7-Bromo-4-(2,4-dimethoxybenzyl)-3,4-dihydro-1H-benzo[e][1,4]diazepine-2,5-dione

HRID 351840ノート

反応式

HRID 351840 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:10][C:9](=[O:11])O[C:7](=[O:12])[C:6]=2[CH:13]=1.[CH3:14][O:15][C:16]1[CH:27]=[C:26]([O:28][CH3:29])[CH:25]=[CH:24][C:17]=1[CH2:18][NH:19][CH2:20]C(O)=O>CC1C=CC(C)=CC=1>[CH3:14][O:15][C:16]1[CH:27]=[C:26]([O:28][CH3:29])[CH:25]=[CH:24][C:17]=1[CH2:18][N:19]1[C:7](=[O:12])[C:6]2[CH:13]=[C:2]([Br:1])[CH:3]=[CH:4][C:5]=2[NH:10][C:9](=[O:11])[CH2:20]1

参加物

4

反応物 2

HCID 2885615-Bromoisatoic AnhydrideHCID 11042399(2,4-Dimethoxy-benzylamino)-acetic acid

生成物 1

HCID 227134707-Bromo-4-(2,4-dimethoxybenzyl)-3,4-dihydro-1H-benzo[e][1,4]diazepine-2,5-dione

試薬・触媒・溶媒 1

HCID 7809P-Xylene溶媒

反応条件

温度
150 °C

実験手順

A suspension of 6-bromo-2H-3,1-bezoxazine-2,4(1H)-dione (22.0 g, 91 mmol) containing (2,4-dimethoxy-benzylamino)-acetic acid (22.5 g, 100 mmol) in p-xylene (200 mL) was heated under reflux (150° C.) for 1 h. After cooling to room temperature the precipitate was filtered off and washed with p-xylene (100 ml). Yield: 33.5 g (91%) m/z 403/405 (M).

後処理

  1. temperaturewas heated
  2. temperatureAfter cooling to room temperature the precipitate
  3. filtrationwas filtered off
  4. washwashed with p-xylene (100 ml)

出典と根拠

ORDレコード
ord-fe179141732e462b91e0f789298484f1
出典データセット
uspto-grants-2004_06
特許番号
US06743789B2

反応ノート

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