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Sodium methanethiolate → 4-Methylsulfanyl-3-(2-m-tolyl-ethoxy)-benzoic acid methyl ester

HRID 2094661
ノート
印刷プレビュー

反応式

HRID 2094661 の反応式
[CH3:1][O:2][C:3](=[O:23])[C:4]1[CH:9]=[CH:8][C:7]([N+]([O-])=O)=[C:6]([O:13][CH2:14][CH2:15][C:16]2[CH:17]=[C:18]([CH3:22])[CH:19]=[CH:20][CH:21]=2)[CH:5]=1.[CH3:24][S-:25].[Na+]>CN1CCN(C)C1=O>[CH3:1][O:2][C:3](=[O:23])[C:4]1[CH:9]=[CH:8][C:7]([S:25][CH3:24])=[C:6]([O:13][CH2:14][CH2:15][C:16]2[CH:17]=[C:18]([CH3:22])[CH:19]=[CH:20][CH:21]=2)[CH:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 4378561Sodium methanethiolateHCID 670764364-Nitro-3-(2-m-tolyl-ethoxy)-benzoic acid methyl ester

生成物 1

HCID 670767584-Methylsulfanyl-3-(2-m-tolyl-ethoxy)-benzoic acid methyl ester収率 66.5%

試薬・触媒・溶媒 1

HCID 66611,3-Dimethyl-2-imidazolidinone溶媒

実験手順

The compound of step 1 (900 mg, 2.85 mmol) was dissolved in 1,3-dimethyl-2-imidazolidinone (6 ml), and sodium methanethiolate (0.23 g, 3.29 mmol) was added. The mixture was reacted at room temperature for 60 h, then partitioned between a saturated sodium chloride solution and EA, and the aqueous phase extracted with EA. The organic extracts were dried over sodium sulfate, filtered and evaporated to dryness. The residue was purified by silica gel chromatography (HEP/EA gradient) to give 600 mg of the title compound.

後処理

  1. customThe mixture was reacted at room temperature for 60 h
  2. custompartitioned between a saturated sodium chloride solution and EA
  3. extractionthe aqueous phase extracted with EA
  4. dry with materialThe organic extracts were dried over sodium sulfate
  5. filtrationfiltered
  6. customevaporated to dryness
  7. customThe residue was purified by silica gel chromatography (HEP/EA gradient)

出典と根拠

ORDレコード
ord-921b3cae3e7041859bd36b352beaacca
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08445530B2

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