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

HRID 606265ノート

反応式

HRID 606265 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-c88eded4398446a2a0e07f62362c7741
出典データセット
uspto-grants-2011_03
特許番号
US07915274B2

反応ノート

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