Sodium amide → 1,5-Dimethyl-1H-1,5-benzodiazepine-2,4(3H,5H)-dione

HRID 1390377

반응식

HRID 1390377 반응식
[NH2-].[Na+].[CH3:3][N:4]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[NH:8][C:7](=[O:15])[CH2:6][C:5]1=[O:16].[CH3:17]OS([O-])(=O)=O>C1(C)C(C)=CC=CC=1>[CH3:3][N:4]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[N:8]([CH3:17])[C:7](=[O:15])[CH2:6][C:5]1=[O:16]

참가 물질

5

반응물 3

HCID 24533Sodium amideHCID 4694097Methyl sulfate(1-)HCID 227492411-methyl 1,2,4,5-tetrahydro 2,4-diketo 3H-1,5-benzodiazepine

생성물 1

HCID 5360091,5-Dimethyl-1H-1,5-benzodiazepine-2,4(3H,5H)-dione

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

2 g of sodium amide are added to a suspension of 9.5 g of 1-methyl 1,2,4,5-tetrahydro 2,4-diketo 3H-1,5-benzodiazepine, obtained in the example XIV, in 30 c.c. of xylene, and the whole is heated for about thirty minutes, while agitating, treated with 20 c.c. of methyl-sulfate and as soon as the exothermic reaction has ceased, this is heated and boiled for three hours. The solvent is evaporated under reduced presure, the residue is taken up in 200 c.c. of a 10% solution of caustic soda, and after agitation, suction filtered, and purified upon crystallisation in 90% ethanol. Yield 4.5 g; melting point: 240°-242° C.

후처리

  1. customobtained in the example XIV, in 30 c.c
  2. additiontreated with 20 c.c
  3. temperaturethis is heated
  4. customThe solvent is evaporated under reduced presure
  5. filtrationof a 10% solution of caustic soda, and after agitation, suction filtered
  6. custompurified upon crystallisation in 90% ethanol

출처 및 근거

ORD 기록
ord-a428d5a73b114d11858602c68098d1fb
출처 데이터셋
uspto-grants-1979_02
특허 번호
US04138572

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