Hydrochloric Acid → 3-Ethoxy-N-[2-(phenylsulfonyl)ethyl]-1-propanamine hydrochloride

HRID 4211

반응식

HRID 4211 반응식
[C:1]1([S:7]([CH2:10][CH2:11][Cl:12])(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:13]([O:15][CH2:16][CH2:17][CH2:18][NH2:19])[CH3:14].C(N(CC)CC)C.Cl>C(#N)C.CO.CCOCC>[ClH:12].[CH2:13]([O:15][CH2:16][CH2:17][CH2:18][NH:19][CH2:11][CH2:10][S:7]([C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1)(=[O:9])=[O:8])[CH3:14]

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 13646((2-Chloroethyl)sulphonyl)benzeneHCID 22720Propanolamine ethyl ether

생성물 1

HCID 136550853-Ethoxy-N-[2-(phenylsulfonyl)ethyl]-1-propanamine hydrochloride수율 63.2%

시약·촉매·용매 3

HCID 887Methanol용매HCID 3283Diethyl Ether용매HCID 6342Acetonitrile용매

실험 절차

A mixture of 51.4 g (0.253 mole) of 2-chloroethyl phenyl sulfone, 50.2 g (0.417 mole) of 3-ethoxy-1-propanamine, and 33.0 g (0.327 mole) of triethylamine in 400 ml of acetonitrile was stirred at room temperature for 20 hr. The solvent was removed in vacuo and the residue was partitioned between methylene chloride and dilute sodium hydroxide. The methylene chloride phase was dried over magnesium sulfate, and the solvent was removed in vacuo to give an oil. This was dissolved in methanol, an excess of ethereal hydrogen chloride was added and ether was added. A precipitate was collected to give 49.2 g (63.2%) of white crystalline solid, m.p. 169°-170° C.

후처리

  1. customThe solvent was removed in vacuo
  2. customthe residue was partitioned between methylene chloride and dilute sodium hydroxide
  3. dry with materialThe methylene chloride phase was dried over magnesium sulfate
  4. customthe solvent was removed in vacuo
  5. customto give an oil
  6. customA precipitate was collected

출처 및 근거

ORD 기록
ord-b9ffe40dfc354894b3753bf7aa940b3d
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04724235

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