5-Methylisatoic anhydride → 3,4-dihydro-3,7-dimethyl-1H-1,4-benzodiazepine-2,5-dione

HRID 326885

반응식

HRID 326885 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.Cl.[NH2:15][CH:16](C)[C:17](OC)=O>N1C=CC=CC=1>[CH3:17][CH:16]1[NH:15][C:7](=[O:12])[C:6]2[CH:13]=[C:2]([CH3:1])[CH:3]=[CH:4][C:5]=2[NH:10][C:9]1=[O:11]

참가 물질

4

반응물 2

HCID 2944785-Methylisatoic anhydrideHCID 2756298Alanine, methyl ester, hydrochloride (1:1)

생성물 1

HCID 212519423,4-dihydro-3,7-dimethyl-1H-1,4-benzodiazepine-2,5-dione수율 50.5%

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
-10 °C

실험 절차

A mixture of 17.7 parts of 6-methyl-4H-3,1-benzoxazine-2,4(1H)-dione, 15.0 parts of methyl 2-aminopropanoate monohydrochloride and 62.7 parts of pyridine was refluxed for 6 hours under argon. The reaction mixture was cooled at -10° C. for 1 hour. The precipitate was filtered off, rinsed with water, triturated in ethanol and rinsed with ethanol and 1,1'-oxybisethane, yielding 10.32 parts (50.5%) of 3,4-dihydro-3,7-dimethyl-1H-1,4-benzodiazepine-2,5-dione (interm. 43).

후처리

  1. temperaturewas refluxed for 6 hours under argon
  2. filtrationThe precipitate was filtered off
  3. washrinsed with water
  4. customtriturated in ethanol
  5. washrinsed with ethanol and 1,1'-oxybisethane

출처 및 근거

ORD 기록
ord-f7165850443545da827498134458d007
출처 데이터셋
uspto-grants-1993_12
특허 번호
US05270464

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