5-Methylisatoic anhydride → 4-(2,4-Dimethoxy-benzyl)-7-methyl-3,4-dihydro-1H-benzo[e][1,4]diazepine-2,5-dione

HRID 351832

반응식

HRID 351832 반응식
[CH3:1][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]([CH3:1])[CH:3]=[CH:4][C:5]=2[NH:10][C:9](=[O:11])[CH2:20]1

참가 물질

4

반응물 2

HCID 2944785-Methylisatoic anhydrideHCID 11042399(2,4-Dimethoxy-benzylamino)-acetic acid

생성물 1

HCID 227135274-(2,4-Dimethoxy-benzyl)-7-methyl-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-methyl-2H-3,1-bezoxazine-2,4(1H)-dione (18.3 g, 103 mmol) containing (2,4-dimethoxy-benzylamino)-acetic acid (25.6 g, 114 mmol) in p-xylene (125 mL) was heated under reflux (150° C.) for 2.5 h. After cooling to room temperature the precipitate was filtered off and washed with p-xylene (2×20 ml). Yield: 34.1 g (97%). m/z 341 (MH+).

후처리

  1. temperaturewas heated
  2. temperatureAfter cooling to room temperature the precipitate
  3. filtrationwas filtered off
  4. washwashed with p-xylene (2×20 ml)

출처 및 근거

ORD 기록
ord-7c28ceb6fdba40719215e231b1ea0bf7
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06743789B2

연결된 노트

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