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Hydrochloric Acid → 3-[4-(3-Chlorophenyl)piperazin-1-yl]propan-1-amine

HRID 373589
ノート
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反応式

HRID 373589 の反応式
Cl.[Cl:2][C:3]1[CH:4]=[C:5]([N:9]2[CH2:14][CH2:13][N:12]([CH2:15][CH2:16][CH2:17][NH:18]C(C3C=CC=CC=3)(C3C=CC=CC=3)C3C=CC=CC=3)[CH2:11][CH2:10]2)[CH:6]=[CH:7][CH:8]=1.CO>O>[Cl:2][C:3]1[CH:4]=[C:5]([N:9]2[CH2:10][CH2:11][N:12]([CH2:15][CH2:16][CH2:17][NH2:18])[CH2:13][CH2:14]2)[CH:6]=[CH:7][CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 19810680HCID 19810680、化合物

生成物 1

HCID 35067593-[4-(3-Chlorophenyl)piperazin-1-yl]propan-1-amine収率 68%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Gaseous hydrochloric acid is introduced for 10 min into a round bottom flask containing 11.2 g (22.6 mmol) of 3-[4-(3-chlorophenyl]piperazin-1-yl]-N-(triphenylmethyl)propanamine and 300 ml of methanol, while the mixture is cooled in a bath of iced water. The mixture is allowed to return to room temperature and is then heated under reflux for 5.5 h. The solution is reduced to half its volume and is allowed to cool. The solid which precipitates is filtered off, is treated with water and aqueous ammonia, the mixture is extracted with ethyl acetate, the organic phase is washed with water and is dried and the solvent is evaporated off. 3.9 g of light yellow oil are obtained.

後処理

  1. customto return to room temperature
  2. temperatureis then heated
  3. temperatureunder reflux for 5.5 h
  4. temperatureto cool
  5. customThe solid which precipitates
  6. filtrationis filtered off
  7. additionis treated with water and aqueous ammonia
  8. extractionthe mixture is extracted with ethyl acetate
  9. washthe organic phase is washed with water
  10. customis dried
  11. customthe solvent is evaporated off

出典と根拠

ORDレコード
ord-847f67f3482f4ecda0dd398ff8783271
出典データセット
uspto-grants-1992_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05164397

反応ノート

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