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

HRID 1414516노트

반응식

HRID 1414516 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 3-H-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 pressure, 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. Analysis: C11H12N2O2Calculated: C % 64.69 H % 5.92; N % 13.72; Found: 64.67; 6.12; 13.95.

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 pressure
  5. filtrationof a 10% solution of caustic soda, and after agitation, suction filtered
  6. custompurified upon crystallisation in 90% ethanol
  7. custom240°-242° C

출처 및 근거

ORD 기록
ord-60b7cf686da64f508159bc57b5ce7afc
출처 데이터셋
uspto-grants-1977_01
특허 번호
US04001408

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