Hydrogen chloride-ethyl acetate → HCID 66732904, compound

HRID 1184643Notes

Reaction equation

HRID 1184643 reaction equation
C(OC(=O)C)C.[ClH:7].[Cl:8][C:9]1[CH:55]=[CH:54][C:12]2[NH:13][CH2:14][CH2:15][CH2:16][CH:17]([O:18][C:19]([CH:21]([N:41]3[CH2:46][CH2:45][N:44](C(OC(C)(C)C)=O)[CH2:43][CH2:42]3)[C:22](=[O:40])[C:23]3[CH:28]=[CH:27][C:26]([NH:29][C:30](=[O:38])[C:31]4[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=4[CH3:37])=[CH:25][C:24]=3[CH3:39])=[O:20])[C:11]=2[CH:10]=1>C(OCC)(=O)C>[ClH:8].[ClH:7].[Cl:8][C:9]1[CH:55]=[CH:54][C:12]2[NH:13][CH2:14][CH2:15][CH2:16][CH:17]([O:18][C:19]([CH:21]([N:41]3[CH2:42][CH2:43][NH:44][CH2:45][CH2:46]3)[C:22](=[O:40])[C:23]3[CH:28]=[CH:27][C:26]([NH:29][C:30](=[O:38])[C:31]4[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=4[CH3:37])=[CH:25][C:24]=3[CH3:39])=[O:20])[C:11]=2[CH:10]=1

Participants

4

Reactant 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 66732885HCID 66732885, compound

Product 1

HCID 66732904HCID 66732904, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

A 4N hydrogen chloride ethyl acetate solution (3.7 ml) was added to an ethyl acetate solution (15 ml) of tert-butyl 4-{7-chloro-1-[2-methyl-4-(2-methyl-benzoylamino)-benzoyl]-2,3,4,5-tetrahydro-1H-benzo[b]azepin-5-yloxycarbonylmethyl}-piperazine-1-carboxylate (1.2 g, 1.8 mmol), and the mixture was stirred at room temperature for 12 hours. The precipitates were collected by filtration, washed with ethyl acetate, and dried to obtain 800 mg of 1-{7-chloro-1-[2-methyl-4-(2-methyl-benzoylamino)-benzoyl]-2,3,4,5-tetrahydro-1H-benzo[b]azepin-5-yloxycarbonylmethyl}-piperazine dihydrochloride as yellow powder.

Workup

  1. filtrationThe precipitates were collected by filtration
  2. washwashed with ethyl acetate
  3. customdried

Sources & evidence

ORD record
ord-9aaea5c506a740fa9c5aa73714e358d0
Source dataset
uspto-grants-2014_03
Patent number
US08669229B2

Reaction notes

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