1,2-Dichloroethane → (1,3-Dihydroisobenzofuran-1-yl)-(piperidin-4-yl)methanone hydrochloride

HRID 890125ノート

反応式

HRID 890125 の反応式
C([N:8]1[CH2:13][CH2:12][CH:11]([C:14]([CH:16]2[C:24]3[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=3)[CH2:18][O:17]2)=[O:15])[CH2:10][CH2:9]1)C1C=CC=CC=1.[Cl:25]CCCl>ClC(OC(Cl)C)=O>[ClH:25].[CH:16]1([C:14]([CH:11]2[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]2)=[O:15])[C:24]2[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=2)[CH2:18][O:17]1

参加物

4

反応物 2

HCID 111,2-DichloroethaneHCID 22248144(1-Benzylpiperidin-4-yl)-(1,3-dihydroisobenzofuran-1-yl)methanone

生成物 1

HCID 22248211(1,3-Dihydroisobenzofuran-1-yl)-(piperidin-4-yl)methanone hydrochloride

試薬・触媒・溶媒 1

HCID 5213051-Chloroethyl chloroformate溶媒

実験手順

After dissolving 517 mg of (1-benzylpiperidin-4-yl)-(1,3-dihydroisobenzofuran-1-yl)methanone in 5 ml of 1,2-dichloroethane, 0.49 ml of 1-chloroethyl chloroformate was added and the mixture was heated to reflux for 1 hour. The reaction solution was distilled off under reduced pressure, 5 ml of methanol was added to the residue and heating to reflux was continued for 1 hour. The reaction solution was distilled off under reduced pressure, saturated aqueous sodium bicarbonate solution was added and extraction was performed with ethyl acetate. The extract was dried over anhydrous magnesium sulfate and then the solvent was distilled off under reduced pressure to obtain 104 mg of (1,3-dihydroisobenzofuran-1-yl)-(piperidin-4-yl)methanone hydrochloride.

後処理

  1. additionwas added
  2. temperaturethe mixture was heated
  3. temperatureto reflux for 1 hour
  4. distillationThe reaction solution was distilled off under reduced pressure, 5 ml of methanol
  5. additionwas added to the residue
  6. temperatureheating
  7. temperatureto reflux
  8. distillationThe reaction solution was distilled off under reduced pressure, saturated aqueous sodium bicarbonate solution
  9. additionwas added
  10. extractionextraction
  11. dry with materialThe extract was dried over anhydrous magnesium sulfate
  12. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-1f1a46e0f9e1432fb07bfb9af7d7d578
出典データセット
uspto-grants-2006_02
特許番号
US06995144B2

反応ノート

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