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

HRID 2247832ノート

反応式

HRID 2247832 の反応式
[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

参加物

4

反応物 2

HCID 87949Lawesson's reagent2 回HCID 103140701-[4-(1-Hexahydroazepinyl)benzenesulphonyl]-2-pyrrolidinone

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-caadda1b07134e45b64f0ace643836ac
出典データセット
uspto-grants-1991_08
特許番号
US05037822

反応ノート

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