Phosphorus oxychloride → HCID 22503253, 화합물

HRID 1251095노트

반응식

HRID 1251095 반응식
[CH2:1]([O:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]1[N+:14]([O-])=[CH:15][C:16]2[C:21]([CH:22]=1)=[CH:20][CH:19]=[CH:18][CH:17]=2)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.P(Cl)(Cl)([Cl:26])=O>>[Cl:26][C:15]1[C:16]2[C:21](=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:22]=[C:13]([CH2:12][CH2:11][CH2:10][CH2:9][O:8][CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[N:14]=1

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 22503278HCID 22503278, 화합물

생성물 1

HCID 22503253HCID 22503253, 화합물

실험 절차

3-(4-Benzyloxybutyl)isoquinoline-2-oxide (2.0 g) and phosphorous oxychloride (5 ml) were reacted at 110° C. for 2 hr.The reaction solution was evaporated, to the resulting residue were added ethyl acetate and aqueous solution of saturated sodium bicarbonate, and the resulting organic layer was washed with water and brine. The organic layer was dried over magnesium sulfate followed by evaporating the solvent. The resulting 1-chloro-3-(4-benzyloxybutyl)isoquinoline obtained as a yellow oil was reacted with N-ethylpiperazine (5 ml) and potassium carbonate (0.5 g) at 120° C. for 5 hr. The reaction solution was then cooled and then partitioned by adding ethyl acetate and water thereto. The resulting organic layer was washe with water and brine, and dried over magnesium sulfate. The solvent was evaporated, and the resulting residue was purified by silica gel column chromatography (methylene chloride/methanol system) to give 1.32 g of the free compound of the title compound as a pale yellow oil.

후처리

  1. customThe reaction solution was evaporated, to the resulting residue
  2. additionwere added ethyl acetate and aqueous solution of saturated sodium bicarbonate
  3. washthe resulting organic layer was washed with water and brine
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. customby evaporating the solvent

출처 및 근거

ORD 기록
ord-4b9d45c688ec4d6fb361537b93c9d75e
출처 데이터셋
uspto-grants-2002_01
특허 번호
US06340759B1

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