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

HRID 4211

反応式

HRID 4211 の反応式
[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]

参加物

8

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 3283Diethyl Ether溶媒HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b9ffe40dfc354894b3753bf7aa940b3d
出典データセット
uspto-grants-1988_02
特許番号
US04724235

関連ノート

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