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Potassium Carbonate → HCID 59565342、化合物

HRID 1962856
ノート
印刷プレビュー

反応式

HRID 1962856 の反応式
[C:1]([C:3]([NH:7][C:8](=[O:30])[CH:9]([S:28][CH3:29])[O:10][C:11]1[CH:12]=[C:13]2[C:18](=[C:19]([CH3:21])[CH:20]=1)[N:17]=[CH:16][C:15]([C:22]#[C:23][Si](C)(C)C)=[CH:14]2)([CH3:6])[CH2:4][F:5])#[N:2].C(=O)([O-])[O-].[K+].[K+].C(=O)([O-])O.[Na+]>CO>[C:1]([C:3]([NH:7][C:8](=[O:30])[CH:9]([O:10][C:11]1[CH:12]=[C:13]2[C:18](=[C:19]([CH3:21])[CH:20]=1)[N:17]=[CH:16][C:15]([C:22]#[CH:23])=[CH:14]2)[S:28][CH3:29])([CH3:6])[CH2:4][F:5])#[N:2]
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 11430Potassium CarbonateHCID 516892Sodium BicarbonateHCID 59565363HCID 59565363、化合物

生成物 1

HCID 59565342HCID 59565342、化合物収率 83%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of N-(1-cyano-2-fluoro-1-methyl-ethyl)-2-methylsulfanyl-2-(8-methyl-3-trimethylsilanylethynyl-quinolin-6-yloxy)-acetamide (685 mg) in methanol (20 mL) was added potassium carbonate (107 mg). The reaction mixture was stirred at room temperature for 15 minutes. The mixture was poured on a saturated solution of sodium hydrogencarbonate and extracted with ethyl acetate (thrice), dried over sodium sulphate, filtered and concentrated under reduced pressure. The crude was purified by chromatography eluting with cyclohexane/ethyl acetate (7:3 by volume), to give N-(1-cyano-2-fluoro-1-methyl-ethyl)-2-(3-ethynyl-8-methyl-quinolin-6-yloxy)-2-methylsulfanyl-acetamide (476 mg) as a white solid.

後処理

  1. extractionextracted with ethyl acetate (thrice)
  2. dry with materialdried over sodium sulphate
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customThe crude was purified by chromatography
  6. washeluting with cyclohexane/ethyl acetate (7:3 by volume)

出典と根拠

ORDレコード
ord-3f4d909271e54c3bb04b2f80b1417c58
出典データセット
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08415272B2

反応ノート

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