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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Lawesson's reagent → HCID 10725969, 화합물

HRID 2395243
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HRID 2395243 반응식
COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:10])=CC=1.[CH3:23][O:24][C:25]([CH:27]1[CH2:31][C:30](=O)[S:29][CH2:28]1)=[O:26]>C1(C)C=CC=CC=1>[CH3:23][O:24][C:25]([CH:27]1[CH2:31][C:30](=[S:10])[S:29][CH2:28]1)=[O:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 87949Lawesson's reagentHCID 10997333HCID 10997333, 화합물

생성물 1

HCID 10725969HCID 10725969, 화합물수율 144.1%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

207 g (0.51 mol) of Lawesson reagent are added at room temperature to a suspension of 149 g (0.93 mol) of tetrahydro-5-oxo-3-thiophenecarboxylic acid methyl ester in 1.23 litres of absolute toluene, and the mixture is boiled at reflux for 16 hours. Then the solvent is removed by distillation in vacuo, the residue is boiled at reflux for 20 minutes four times in one litre of a solvent mixture of petroleum ether and diethyl ether 1:1 each time, and the extract phase is in each case decanted off and concentrated. After distillation of the crude substance at 130°-140° C./0.03 mbar using a bulb tube, 129.5 g of orange oil are obtained.

후처리

  1. temperatureat reflux for 16 hours
  2. customThen the solvent is removed by distillation in vacuo
  3. temperatureat reflux for 20 minutes four times
  4. additionin one litre of a solvent mixture of petroleum ether and diethyl ether 1:1 each time
  5. customdecanted off
  6. concentrationconcentrated
  7. distillationAfter distillation of the crude substance at 130°-140° C./0.03 mbar

출처 및 근거

ORD 기록
ord-62d61c60a3cc497a87d204ddfec8e018
출처 데이터셋
uspto-grants-1998_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05814629

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