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Cesium carbonate → Methyl 4-chloro-3-cyclopropylmethylthio-2-methylbenzoate

HRID 548591
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HRID 548591 반응식
C(=O)([O-])[O-].[Cs+].[Cs+].[Cl:7][C:8]1[CH:17]=[CH:16][C:11]([C:12]([O:14][CH3:15])=[O:13])=[C:10]([CH3:18])[C:9]=1[SH:19].[CH:20]1([CH2:23]Br)[CH2:22][CH2:21]1>C(#N)C>[Cl:7][C:8]1[CH:17]=[CH:16][C:11]([C:12]([O:14][CH3:15])=[O:13])=[C:10]([CH3:18])[C:9]=1[S:19][CH2:23][CH:20]1[CH2:22][CH2:21]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 81503BromomethylcyclopropaneHCID 67158973Methyl 4-chloro-3-mercapto-2-methylbenzoate

생성물 1

HCID 67158113Methyl 4-chloro-3-cyclopropylmethylthio-2-methylbenzoate

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

1.66 g (5.09 mmol) of cesium carbonate in 20 ml of acetonitrile were added to 1.05 g (4.85 mmol) of methyl 4-chloro-3-mercapto-2-methylbenzoate. 687 mg (5.09 mmol) of cyclopropylmethyl bromide were slowly added dropwise, and the reaction mixture was stirred at RT for 16 h. For work-up, the solvent was removed, and water was added to the residue. The mixture was extracted three times with ethyl acetate, the combined organic phases were dried and filtered and the solvent was removed. What was isolated were 1.2 g of pure product.

후처리

  1. customFor work-up, the solvent was removed
  2. additionwater was added to the residue
  3. extractionThe mixture was extracted three times with ethyl acetate
  4. customthe combined organic phases were dried
  5. filtrationfiltered
  6. customthe solvent was removed
  7. customWhat was isolated

출처 및 근거

ORD 기록
ord-8ebbb95c94ea4562a6fc248714bd1edf
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07943551B2

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