Hydrochloric Acid → HCID 66930789, compound

HRID 1364135Notes

Reaction equation

HRID 1364135 reaction equation
[N:1]1([C:6]2[CH:11]=[CH:10][C:9]([N:12]3[CH:21]=[C:20]4[C:14]([CH2:15][CH2:16][N:17](C(OC(C)(C)C)=O)[CH2:18][CH2:19]4)=[N:13]3)=[CH:8][CH:7]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1.Cl>O1CCOCC1.CO>[N:1]1([C:6]2[CH:11]=[CH:10][C:9]([N:12]3[CH:21]=[C:20]4[C:14]([CH2:15][CH2:16][NH:17][CH2:18][CH2:19]4)=[N:13]3)=[CH:8][CH:7]=2)[CH2:2][CH2:3][CH2:4][CH2:5]1

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 66930909HCID 66930909, compound

Product 1

HCID 66930789HCID 66930789, compound

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 312751,4-DioxaneSolvent2×

Procedure

To a solution of 1,1-dimethylethyl 2-[4-(1-pyrrolidinyl)phenyl]-4,5,7,8-tetrahydropyrazolo[3,4-d]azepine-6(2H)-carboxylate (may be prepared as described in Description 44) (79 mg, 0.21 mmol) in dioxan (3 ml) was added 4M hydrochloric acid in dioxan (2 ml). The resulting mixture was stirred at room temperature, under argon, overnight. The reaction mixture was diluted with methanol and then purified by SCX, eluting with methanol and then 2M ammonia/methanol. The basic fractions were combined and solvent evaporated in vacuo to afford the title compound (D45). MS (ES+) m/e 283 [M+H]+.

Workup

  1. custompurified by SCX
  2. washeluting with methanol
  3. customsolvent evaporated in vacuo

Sources & evidence

ORD record
ord-a92e6459b2e143d5b7edd1fdc09025ac
Source dataset
uspto-grants-2011_02
Patent number
US07888347B2

Reaction notes

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