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

HRID 351840노트

반응식

HRID 351840 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 7809P-Xylene용매

반응 조건

온도
150 °C

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-fe179141732e462b91e0f789298484f1
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06743789B2

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