HCID 178521662, compound → HCID 178478520, compound

HRID 1965971Notes

Reaction equation

HRID 1965971 reaction equation
[Cl:1][C:2]1[CH:18]=[CH:17][C:5]2[CH2:6][CH2:7][N:8](C(=O)C(F)(F)F)[CH2:9][CH2:10][C:4]=2[C:3]=1[C:19]1[NH:20][N:21]=[N:22][C:23]=1[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>N.CO>[ClH:1].[Cl:1][C:2]1[CH:18]=[CH:17][C:5]2[CH2:6][CH2:7][NH:8][CH2:9][CH2:10][C:4]=2[C:3]=1[C:19]1[NH:20][N:21]=[N:22][C:23]=1[C:24]1[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=1

Participants

4

Reactant 1

HCID 178521662HCID 178521662, compound

Product 1

HCID 178478520HCID 178478520, compoundYield 193.8%

Reagents, catalysts & solvents 2

HCID 222AmmoniaSolventHCID 887MethanolSolvent

Procedure

Stir 7-chloro-6-(5-phenyl-3H-[1,2,3]triazol-4-yl)-3-(2,2,2-trifluoroacetyl)-2,3,4,5-tetrahydro-1H-benzo[d]azepine (43 mg, 0.1 mmol) in 7M ammonia in methanol (10 mL) for 16 h. Concentrate the mixture in vacuo, and purify the residue by SCX chromatography. Use a method similar to the General Procedure 2-2 to obtain the desired intermediate (35 mg, 97%). MS (ES+) m/z: 325 (M+H)+.

Workup

  1. concentrationConcentrate the mixture in vacuo
  2. custompurify the residue by SCX chromatography

Sources & evidence

ORD record
ord-950c7bd1937b46c9b16098e2a6e1b56d
Source dataset
uspto-grants-2013_04
Patent number
US08420631B2

Reaction notes

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