Hydrochloric Acid → HCID 9861328, compound

HRID 1955341Notes

Reaction equation

HRID 1955341 reaction equation
[C:1]([C:3]1[CH:20]=[CH:19][C:6]([O:7][CH2:8][CH2:9][CH2:10][N:11]2[CH2:16][CH:15]3[CH2:17][CH2:18][CH:12]2[CH2:13][CH2:14]3)=[CH:5][CH:4]=1)#[CH:2].[ClH:21]>C(OCC)(=O)C.CO.C(OCC)C>[ClH:21].[C:1]([C:3]1[CH:4]=[CH:5][C:6]([O:7][CH2:8][CH2:9][CH2:10][N:11]2[CH2:16][CH:15]3[CH2:14][CH2:13][CH:12]2[CH2:18][CH2:17]3)=[CH:19][CH:20]=1)#[CH:2]

Participants

6

Reactant 2

HCID 313Hydrochloric AcidHCID 9861329HCID 9861329, compound

Product 1

HCID 9861328HCID 9861328, compound

Reagents, catalysts & solvents 3

HCID 887MethanolSolventHCID 3283Diethyl EtherSolventHCID 8857Ethyl AcetateSolvent

Procedure

A solution of compound 9 (0.238 g) in ethyl acetate (2 ml) and methanol (4 ml), under cooling to a solution, was treated with HCl gas in ethyl ether dropwise to adjust the pH 5.0, then concentrated in vacuo. The concentrate was crystallized with ethyl acetate. The resulting precipitate was collected by filtration, and was recrystallized with ethyl acetate. Compound 10 was obtained as a pale yellow crystal(0.172 g).

Workup

  1. concentrationconcentrated in vacuo
  2. customThe concentrate was crystallized with ethyl acetate
  3. filtrationThe resulting precipitate was collected by filtration
  4. customwas recrystallized with ethyl acetate

Sources & evidence

ORD record
ord-4423e39131e2427d865f274eb9da448b
Source dataset
uspto-grants-2000_09
Patent number
US06124460

Reaction notes

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