Hydrochloric Acid → HCID 131722787, compound

HRID 1386521Notes

Reaction equation

HRID 1386521 reaction equation
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]([CH:24]([CH3:26])[CH3:25])([CH2:11][CH2:12][CH:13]([N:15]([CH3:23])[CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)C)[C:9]#[N:10].[ClH:27]>CO>[ClH:27].[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]([CH:24]([CH3:26])[CH3:25])([CH2:11][CH2:12][CH2:13][N:15]([CH3:23])[CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[C:9]#[N:10]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 21181564HCID 21181564, compound

Product 1

HCID 131722787HCID 131722787, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent2×

Procedure

A solution of the product of Example 8, Step (c) (470 mg) in methanol (10 mL) was acidified with a solution of hydrochloric acid in methanol. The solvent was evaporated, and the residue was dried by azeotropic distillation with toluene. Crystallization of the residue from ethyl acetate gave the title compound (333 mg) as a white, crystalline solid, m.p. 164° C., characterized as follows: Analysis for C22H28FN2Cl (MW 374.93); Calc'd: C, 70.47; H, 7.53; N, 7.47; Found: C, 70.36; H, 7.54; N, 7.42.

Workup

  1. customThe solvent was evaporated
  2. dry with materialthe residue was dried by azeotropic distillation with toluene
  3. customCrystallization of the residue from ethyl acetate

Sources & evidence

ORD record
ord-003bd051999c4d1fabb58087ef49d3e2
Source dataset
uspto-grants-2001_07
Patent number
US06265439B1

Reaction notes

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