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

HRID 548591
ノート
印刷プレビュー

反応式

HRID 548591 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8ebbb95c94ea4562a6fc248714bd1edf
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07943551B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート