Lawesson's reagent → 1-[4-(1-Hexahydroazepinyl)benzenesulphonyl]-2-pyrrolidinethione

HRID 2247832노트

반응식

HRID 2247832 반응식
[N:1]1([C:8]2[CH:13]=[CH:12][C:11]([S:14]([N:17]3[CH2:21][CH2:20][CH2:19][C:18]3=O)(=[O:16])=[O:15])=[CH:10][CH:9]=2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:32])=CC=1>O1CCCC1>[N:1]1([C:8]2[CH:13]=[CH:12][C:11]([S:14]([N:17]3[CH2:21][CH2:20][CH2:19][C:18]3=[S:32])(=[O:16])=[O:15])=[CH:10][CH:9]=2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

참가 물질

4

반응물 2

HCID 87949Lawesson's reagent2회HCID 103140701-[4-(1-Hexahydroazepinyl)benzenesulphonyl]-2-pyrrolidinone

생성물 1

HCID 103597991-[4-(1-Hexahydroazepinyl)benzenesulphonyl]-2-pyrrolidinethione

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture comprising 12.53 g of 1-[4-(1-hexahydroazepinyl)benzenesulphonyl]-2-pyrrolidinone, prepared as in Example 18 of the European Patent published under No. 0,033,578, and 7.5 g of Lawesson reagent (or 2,4-bis(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane 2,4-disulphide) in 250 cm3 of tetrahydrofuran is heated to reflux for 48 hours. The mixture is allowed to return to room temperature and is evaporated to dryness, and the residue is chromatographed on silica (eluant: benzene). 7.3 g of product are recovered. M.p. 173°-175° C. After crystallization in a chloroform/n-hexane mixture, 6 g of expected pure product are obtained. M.p. 176°-178° C.

후처리

  1. temperatureto reflux for 48 hours
  2. customto return to room temperature
  3. customis evaporated to dryness
  4. customthe residue is chromatographed on silica (eluant: benzene)
  5. custom7.3 g of product are recovered
  6. customAfter crystallization in a chloroform/n-hexane mixture, 6 g of expected pure product
  7. customare obtained

출처 및 근거

ORD 기록
ord-caadda1b07134e45b64f0ace643836ac
출처 데이터셋
uspto-grants-1991_08
특허 번호
US05037822

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