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Hydrochloric Acid → HCID 70619308, 화합물

HRID 616204
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HRID 616204 반응식
[CH2:1]([O:3][C:4]([C:6]1([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH2:11][CH2:10][N:9]([CH2:12][CH2:13]O)[CH2:8][CH2:7]1)=[O:5])[CH3:2].[ClH:21].S(Cl)([Cl:24])=O>C(Cl)Cl>[ClH:24].[CH2:1]([O:3][C:4]([C:6]1([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH2:11][CH2:10][N:9]([CH2:12][CH2:13][Cl:21])[CH2:8][CH2:7]1)=[O:5])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 24386Thionyl ChlorideHCID 21389218Ethyl 1-(2-hydroxyethyl)-4-phenylpiperidine-4-carboxylate

생성물 1

HCID 70619308HCID 70619308, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution is prepared from 5.9 parts of the ester obtained in the preceding paragraph and 134 parts of methylene chloride. This solution is saturated with hydrogen chloride gas at below 10° and 5.1 parts of thionyl chloride is added. The mixture is refluxed for 1 hour and then cooled and volatile material is removed under reduced pressure. The residue is dissolved in 88 parts of benzene, and the solution evaporated under reduced pressure. The residue is then crystallized from a mixture of ethanol and ether to give 1-(2-chloroethyl)-4-phenyl-4-piperidinecarboxylic acid ethyl ester hydrochloride melting at about 216°-218°.

후처리

  1. temperatureThe mixture is refluxed for 1 hour
  2. temperaturecooled
  3. customvolatile material is removed under reduced pressure
  4. dissolutionThe residue is dissolved in 88 parts of benzene
  5. customthe solution evaporated under reduced pressure
  6. customThe residue is then crystallized from a mixture of ethanol and ether

출처 및 근거

ORD 기록
ord-8c77007ecd3649eb9c2582f09e57741e
출처 데이터셋
uspto-grants-1978_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04072686

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