Sarcosine → 3,4-dihydro-4,6-dimethyl-2H-1,4-benzodiazepine-2,5(1H)-dione

HRID 67375

반응식

HRID 67375 반응식
[CH3:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[NH:12][C:11](=[O:13])O[C:8](=[O:9])[C:7]=12.[NH:14]([CH2:16]C(O)=O)[CH3:15]>CS(C)=O>[CH3:15][N:14]1[C:8](=[O:9])[C:7]2[C:2]([CH3:1])=[CH:3][CH:4]=[CH:5][C:6]=2[NH:12][C:11](=[O:13])[CH2:16]1

참가 물질

4

반응물 2

HCID 1088SarcosineHCID 104875225-methyl-2,4-dihydro-1H-3,1-benzoxazine-2,4-dione

생성물 1

HCID 217089753,4-dihydro-4,6-dimethyl-2H-1,4-benzodiazepine-2,5(1H)-dione

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

반응 조건

온도
110 °C

실험 절차

A mixture of 14.0 g (79 mmol) of 6-methylisatoic acid anhydride, 7.04 g (79 mmol) of sarcosine and 80 ml of dimethyl sulphoxide is stirred at 110° C. for 3 hours. The red coloured solution is evaporated in a high vacuum. The residue is treated with 80 ml of ethanol, the product crystallising out. There is obtained 3,4-dihydro-4,6-dimethyl-2H-1,4-benzodiazepine-2,5(1H)-dione of melting point 200°-202° C.

후처리

  1. customThe red coloured solution is evaporated in a high vacuum
  2. additionThe residue is treated with 80 ml of ethanol
  3. customthe product crystallising out

출처 및 근거

ORD 기록
ord-3182e92f9292405e8150e0d2d9c7d3f1
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04346031

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