Iodoethane → HCID 66885794, compound

HRID 1500568Notes

Reaction equation

HRID 1500568 reaction equation
[S:1]1[CH:5]=[CH:4][C:3]2[C:6]([N:10]3[CH2:15][CH2:14][N:13]([CH2:16][CH2:17][CH2:18][O:19][C:20]4[CH:29]=[C:28]5[C:23]([CH2:24][CH2:25][N:26]([CH2:31][CH3:32])[C:27]5=[O:30])=[CH:22][CH:21]=4)[CH2:12][CH2:11]3)=[CH:7][CH:8]=[CH:9][C:2]1=2.S1C=CC2C(N3CCN(CCCOC4C=C5C(CCNC5=O)=CC=4)CC3)=CC=CC1=2.C(I)C.CO.[ClH:68]>CO>[ClH:68].[ClH:68].[S:1]1[CH:5]=[CH:4][C:3]2[C:6]([N:10]3[CH2:11][CH2:12][N:13]([CH2:16][CH2:17][CH2:18][O:19][C:20]4[CH:29]=[C:28]5[C:23]([CH2:24][CH2:25][N:26]([CH2:31][CH3:32])[C:27]5=[O:30])=[CH:22][CH:21]=4)[CH2:14][CH2:15]3)=[CH:7][CH:8]=[CH:9][C:2]1=2

Participants

6

Reactant 4

HCID 6340IodoethaneHCID 11978818HCID 11978818, compoundHCID 21893726Hydrochloride methanolHCID 66885795HCID 66885795, compound

Product 1

HCID 66885794HCID 66885794, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

By a similar method as in Example 18, 7-[3-(4-benzo[b]thiophen-4-yl-piperazin-1-yl)propoxy]-2-ethyl-3,4-dihydro-2H-isoquinolin-1-one was prepared from 7-[3-(4-benzo[b]thiophen-4-yl-piperazin-1-yl)propoxy]-3,4-dihydro-2H-isoquinolin-1-one using ethyl iodide, and after it was made into a methanol solution, 0.5N hydrochloric acid methanol solution was added thereto, precipitated crystals were separated by filtration, recrystallized from a mixed solvent of methanol-ethyl acetate and thereby 7-[3-(4-benzo[b]thiophen-4-yl-piperazin-1-yl)propoxy]-2-ethyl-3,4-dihydro-2H-isoquinolin-1-one dihydrochloride was obtained in the form of a white powder.

Workup

  1. additionwas added
  2. customprecipitated crystals
  3. customwere separated by filtration
  4. customrecrystallized from a mixed solvent of methanol-ethyl acetate

Sources & evidence

ORD record
ord-650a78b109104c8eb8beeec4ade62408
Source dataset
uspto-grants-2015_12
Patent number
US09206167B2

Reaction notes

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