Oxalic Acid → N,N-Diethyl-N'-[2-(phenylsulfonyl)ethyl]-1,4-butanediamine oxalate hydrate

HRID 330398

반응식

HRID 330398 반응식
Cl[CH2:2][CH2:3][S:4]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)(=[O:6])=[O:5].[CH2:13]([N:15]([CH2:18][CH2:19][CH2:20][CH2:21][NH2:22])[CH2:16][CH3:17])[CH3:14].[C:23]([OH:28])(=[O:27])[C:24]([OH:26])=[O:25]>C(#N)C>[OH2:5].[C:23]([OH:28])(=[O:27])[C:24]([OH:26])=[O:25].[CH2:13]([N:15]([CH2:16][CH3:17])[CH2:18][CH2:19][CH2:20][CH2:21][NH:22][CH2:2][CH2:3][S:4]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)(=[O:6])=[O:5])[CH3:14]

참가 물질

5

반응물 3

HCID 971Oxalic AcidHCID 13646((2-Chloroethyl)sulphonyl)benzeneHCID 117976N,N-Diethyl-1,4-butanediamine

생성물 1

HCID 19869533N,N-Diethyl-N'-[2-(phenylsulfonyl)ethyl]-1,4-butanediamine oxalate hydrate수율 164.4%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 28.2 g (0.138 mole) of [(2-chloroethyl)sulfonyl]benzene and 20.0 g (0.139 mole) of 4-(N,N-diethylamino)-1-butanamine in 700 ml of acetonitrile was stirred at room temperature for 16 hr. The solvent was removed in vacuo, and the residue was partitioned between methylene chloride and dilute sodium hydroxide. The methylene chloride solution was dried over magnesium sulfate, and the solvent was removed in vacuo. The residue was dissolved in methanol, a solution of 25.0 g (0.278 mole) of oxalic acid was added and a precipitate was collected to give 47.69 g (68.9%) of title compound, a white crystalline solid, mp 158°-165° C. with decomposition.

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 solution was dried over magnesium sulfate
  4. customthe solvent was removed in vacuo
  5. dissolutionThe residue was dissolved in methanol
  6. customa precipitate was collected

출처 및 근거

ORD 기록
ord-c6dccbefbc6a4abbadf02e99b7bdf981
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04895840

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