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

HRID 1414516

反応式

HRID 1414516 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-60b7cf686da64f508159bc57b5ce7afc
出典データセット
uspto-grants-1977_01
特許番号
US04001408

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