Iodine → 4,5-dihydro-3-iodo-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one

HRID 223215노트

반응식

HRID 223215 반응식
[CH3:1][N:2]1[C:8](=[O:9])[C:7]2[CH:10]=[CH:11][CH:12]=[CH:13][C:6]=2[N:5]2[CH:14]=[N:15][CH:16]=[C:4]2[CH2:3]1.[I:17]I.O>CN(C)C=O>[I:17][C:16]1[N:15]=[CH:14][N:5]2[C:6]3[CH:13]=[CH:12][CH:11]=[CH:10][C:7]=3[C:8](=[O:9])[N:2]([CH3:1])[CH2:3][C:4]=12

참가 물질

5

반응물 3

HCID 807IodineHCID 962WaterHCID 199051164,5-dihydro-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one

생성물 1

HCID 198306774,5-dihydro-3-iodo-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1.06 g (5 mmol) of 4,5-dihydro-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one are stirred at 90° for 40 hours together with 1.26 g of iodine in 20 ml of dimethylformamide. The mixture is poured into water and extracted three times with chloroform. The chloroform extracts are washed five times with water, dried over magnesium sulphate and evaporated. By chromatography of the residue on a silica gel column there is obtained 4,5-dihydro-3-iodo-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one of melting point 174°-176°.

후처리

  1. extractionextracted three times with chloroform
  2. washThe chloroform extracts are washed five times with water
  3. dry with materialdried over magnesium sulphate
  4. customevaporated

출처 및 근거

ORD 기록
ord-074f7ea76dc64524b5e16a283434949b
출처 데이터셋
uspto-grants-1982_10
특허 번호
US04352818

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