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Hexane → HCID 19783086, 화합물

HRID 257338
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HRID 257338 반응식
[F:1][C:2]1([C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:7][CH2:6][CH2:5][CH2:4][C:3]1=O.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:23])=CC=1.CCCCCC>C1(C)C=CC=CC=1>[F:1][C:2]1([C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:7][CH2:6][CH2:5][CH:4]=[C:3]1[SH:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8058HexaneHCID 87949Lawesson's reagentHCID 10921276Ethyl 1-fluoro-2-oxocyclohexanecarboxylate

생성물 1

HCID 19783086HCID 19783086, 화합물수율 18%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Referring to the process described in Bulletin des Societe Chimiques Belges volume 87, page 223 (1978), 5.4 g (30 mmol) of ethyl 1-fluoro-2-oxocyclohexanecarboxylate was dissolved in 50 ml of toluene, to this was added 6.0 g (15 mmol) of Lawesson's reagent, and reaction was carried out at 100° C. for 5 hours. 100 ml of hexane was added, the precipitate was filtered out and the solvent was distilled away. The filtrate was purified by silica gel column chromatography (developing solvent: hexane / ethyl acetate=15/1) to obtain 1.1 g (yield: 18 % of ethyl 1-fluoro-2-mercapto-2-cyclohexenecarboxylate.

후처리

  1. additionto this was added
  2. filtrationthe precipitate was filtered out
  3. distillationthe solvent was distilled away
  4. customThe filtrate was purified by silica gel column chromatography (developing solvent: hexane / ethyl acetate=15/1)

출처 및 근거

ORD 기록
ord-b4997bd2b13145f382fa1fd4454cd9c4
출처 데이터셋
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05262385

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