Dimethylformamide diethylacetal → HCID 54171996, compound

HRID 1076394Notes

Reaction equation

HRID 1076394 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[C:16]([I:19])[CH:17]=[CH:18][C:13]=2[N:12]([CH3:20])[C:11](=[O:21])[CH2:10][N:9]=1.C(O[CH:25](OCC)[N:26]([CH3:28])[CH3:27])C>>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[C:16]([I:19])[CH:17]=[CH:18][C:13]=2[N:12]([CH3:20])[C:11](=[O:21])[C:10](=[CH:25][N:26]([CH3:28])[CH3:27])[N:9]=1

Participants

3

Reactant 2

HCID 70913Dimethylformamide diethylacetalHCID 21540282HCID 21540282, compound

Product 1

HCID 54171996HCID 54171996, compound

Conditions

Temperature
130 °C

Procedure

A mixture consisting of 8 gm of 5-(2'-chloro-phenyl)-1,3-dihydro-7-iodo-1-methyl-2H-1,4-benzodiazepin-2-one and 16 ml of N,N-dimethyl-formamide-diethylacetal was heated for 90 minutes at 130°C. Thereafter, the reaction mixture was allowed to cool, and the crystalline substance which separated out was collected by vacuum filtration and washed with benzene and petroleum ether, yielding the compound named in the heading, which had a melting point of 182°-184°C.

Workup

  1. temperatureto cool
  2. customthe crystalline substance which separated out
  3. filtrationwas collected by vacuum filtration
  4. washwashed with benzene and petroleum ether
  5. customyielding the compound

Sources & evidence

ORD record
ord-ac2a9f5cb3434860bec13b9f32978b5b
Source dataset
uspto-grants-1976_05
Patent number
US03956492

Reaction notes

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