Phosphorus oxychloride → HCID 22503253、化合物

HRID 1006866ノート

反応式

HRID 1006866 の反応式
[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

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 22503278HCID 22503278、化合物

生成物 1

HCID 22503253HCID 22503253、化合物

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-681fb69783c84e27b5000493a0a79176
出典データセット
uspto-grants-2004_09
特許番号
US06790844B2

反応ノート

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