4-Chlorophenylacetyl chloride → HCID 15614776, compound

HRID 1084584Notes

Reaction equation

HRID 1084584 reaction equation
[NH2:1][CH:2]1[N:8]=[C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[C:6]2[CH:15]=[CH:16][CH:17]=[CH:18][C:5]=2[N:4]([CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21])[C:3]1=[O:25].[Cl:26][C:27]1[CH:32]=[CH:31][C:30]([CH2:33][C:34](Cl)=[O:35])=[CH:29][CH:28]=1>>[CH2:23]([O:22][C:20](=[O:21])[CH2:19][N:4]1[C:5]2[CH:18]=[CH:17][CH:16]=[CH:15][C:6]=2[C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[N:8][CH:2]([NH:1][C:34](=[O:35])[CH2:33][C:30]2[CH:31]=[CH:32][C:27]([Cl:26])=[CH:28][CH:29]=2)[C:3]1=[O:25])[CH3:24]

Participants

3

Reactant 2

HCID 906924-Chlorophenylacetyl chlorideHCID 10065651HCID 10065651, compound

Product 1

HCID 15614776HCID 15614776, compound

Procedure

The procedure of Example 134 was carried out using equivalent amounts of 3(R,S)-amino-1,3-dihydro-1-ethoxycarbonylmethyl-5-phenyl-2H-1,4-benzodiazepin-2-one and 4-chlorophenylacetyl chloride. The product was purified by chromatography on silica gel (hexane-ethyl acetate elution). The combined product fractions were evaporated to dryness in vacuo and crystallized to give the title compound which was dried at 65° C.: m.p. 205°-207° C.

Workup

  1. customThe product was purified by chromatography on silica gel (hexane-ethyl acetate elution)
  2. customThe combined product fractions were evaporated to dryness in vacuo
  3. customcrystallized

Sources & evidence

ORD record
ord-093de365a1534dfda27aae281dd85b9b
Source dataset
uspto-grants-1991_04
Patent number
US05004741

Reaction notes

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