Hydrochloric Acid → 2-[3-(3,4-Dichlorophenyl)piperidin-3-yl]ethanol

HRID 742630ノート

反応式

HRID 742630 の反応式
Cl.O1CCCCC1[O:8][CH2:9][CH2:10][C:11]1([C:17]2[CH:22]=[CH:21][C:20]([Cl:23])=[C:19]([Cl:24])[CH:18]=2)[CH2:16][CH2:15][CH2:14][NH:13][CH2:12]1>CCOCC.CO.C(OC(C)C)(C)C.CCOCC>[OH:8][CH2:9][CH2:10][C:11]1([C:17]2[CH:22]=[CH:21][C:20]([Cl:23])=[C:19]([Cl:24])[CH:18]=2)[CH2:16][CH2:15][CH2:14][NH:13][CH2:12]1

参加物

6

反応物 2

HCID 313Hydrochloric AcidHCID 211976913-(2-Tetrahydropyranyloxyethyl)-3-(3,4-dichlorophenyl)piperidine

生成物 1

HCID 154604002-[3-(3,4-Dichlorophenyl)piperidin-3-yl]ethanol収率 106.9%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 3283Diethyl Ether溶媒HCID 21919906Ether isopropyl ether溶媒

実験手順

A saturated solution of hydrogen chloride in ether is added to a solution of 55 g of 3-(2-tetrahydropyranyloxyethyl)-3-(3,4-dichlorophenyl)piperidine in 200 ml of methanol until the pH is 1. The mixture is stirred for half an hour at room temperature and concentrated to dryness, the residue is taken up in water, rendered alkaline with a solution of NaOH and extracted with CH2Cl2 and the extract is washed with a saturated solution of. NaCl, dried over Na2SO4 and evaporated to dryness to give an oil. This oil is taken up in 200 ml of an isopropyl ether/ether mixture (50/50 v/v). After stirring and filtration, the product is washed with ethyl ether and dried under vacuum over P2O5 to give 45 g of the expected product. M.p.=22° C.

後処理

  1. concentrationconcentrated to dryness
  2. extractionextracted with CH2Cl2
  3. washthe extract is washed with a saturated solution of
  4. dry with materialNaCl, dried over Na2SO4
  5. customevaporated to dryness
  6. customto give an oil
  7. stirringAfter stirring
  8. filtrationfiltration
  9. washthe product is washed with ethyl ether
  10. dry with materialdried under vacuum over P2O5

出典と根拠

ORDレコード
ord-109334a696ed47129d5cbe852783e924
出典データセット
uspto-grants-1996_09
特許番号
US05554763

反応ノート

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