1-Chloroethyl chloroformate → 4-Piperidinecarbonitrile hydrochloride

HRID 47331

反応式

HRID 47331 の反応式
C([N:8]1[CH2:13][CH2:12][CH:11]([C:14]#[N:15])[CH2:10][CH2:9]1)C1C=CC=CC=1.[Cl:16]C(OC(Cl)C)=O>ClCCCl>[ClH:16].[NH:8]1[CH2:13][CH2:12][CH:11]([C:14]#[N:15])[CH2:10][CH2:9]1

参加物

4

反応物 2

HCID 5213051-Chloroethyl chloroformateHCID 7933831-Benzylpiperidine-4-carbonitrile

生成物 1

HCID 227446374-Piperidinecarbonitrile hydrochloride

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

11.0 g of 1-benzyl-4-piperidinecarbonitrile was dissolved in 100 ml 1,2-dichloroethane, 7.1 ml 1-chloroethyl chloroformate was added thereto under ice-cooling. The mixture was stirred at room temperature for 15 min, and then heated under reflux for 1 hr and 20 min. After evaporating, 50 ml methanol was added thereto and it was heated under reflux for 1 hr. The reaction solution was evaporated, and the crystalline residue was washed with ethyl acetate and collected by filtration to give 8.0 g of 4-piperidinecarbonitrile hydrochloride as white crystals.

後処理

  1. temperatureunder ice-cooling
  2. temperatureheated
  3. temperatureunder reflux for 1 hr and 20 min
  4. customAfter evaporating
  5. addition50 ml methanol was added
  6. temperatureit was heated
  7. temperatureunder reflux for 1 hr
  8. customThe reaction solution was evaporated
  9. washthe crystalline residue was washed with ethyl acetate
  10. filtrationcollected by filtration

出典と根拠

ORDレコード
ord-9abad2bad37b48f4ac33a04be491986d
出典データセット
uspto-grants-2004_03
特許番号
US06699870B2

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