Lawesson's reagent → HCID 86727413, 화합물

HRID 519048노트

반응식

HRID 519048 반응식
[N+:1]([C:4]1[CH:21]=[CH:20][C:7]2[S:8][CH2:9][C:10](=O)[N:11]([CH:12]([CH3:18])[C:13]([O:15][CH2:16][CH3:17])=[O:14])[C:6]=2[CH:5]=1)([O-:3])=[O:2].COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:31])=CC=1>C1(C)C=CC=CC=1>[N+:1]([C:4]1[CH:21]=[CH:20][C:7]2[S:8][CH2:9][C:10](=[S:31])[N:11]([CH:12]([CH3:18])[C:13]([O:15][CH2:16][CH3:17])=[O:14])[C:6]=2[CH:5]=1)([O-:3])=[O:2]

참가 물질

4

반응물 2

HCID 87949Lawesson's reagentHCID 86727412HCID 86727412, 화합물

생성물 1

HCID 86727413HCID 86727413, 화합물수율 55%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of ethyl 2-(6-nitro-3-oxo-2H-benzo[b][1,4]thiazin-4(3H)-yl)propanoate (0.189 g, 0.61 mmol) and Lawesson's reagent (0.493 g, 1.22 mmol) in toluene (40 mL) was heated at reflux for 16 h. After cooling to ambient temperature, the mixture was concentrated in vacuo. The residue was purified by column chromatography on silica gel (eluting with 8% EtOAc in petroleum ether) to give ethyl 2-(6-nitro-3-thioxo-2H-benzo[b][1,4]thiazin-4(3H)-yl)propanoate (0.109 g, 55%). TLC (eluting with 25% EtOAc in petroleum ether) Rf=0.3.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 16 h
  3. concentrationthe mixture was concentrated in vacuo
  4. customThe residue was purified by column chromatography on silica gel (eluting with 8% EtOAc in petroleum ether)

출처 및 근거

ORD 기록
ord-4d12e645288545edb002e919f55eedac
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09115151B2

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