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Potassium Carbonate → HCID 178437996、化合物

HRID 1520002
ノート
印刷プレビュー

反応式

HRID 1520002 の反応式
C(=O)([O-])[O-].[K+].[K+].C[Si]([C:11]#[C:12][C:13]1[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[N:15](C(OC(C)(C)C)=O)[N:14]=1)(C)C>CCO>[C:12]([C:13]1[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[NH:15][N:14]=1)#[CH:11]
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 11430Potassium CarbonateHCID 67981125tert-butyl 3-((trimethylsilyl)ethynyl)-1H-indazole-1-carboxylate

生成物 1

HCID 178437996HCID 178437996、化合物収率 80%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Potassium carbonate (880 mg, 6.4 mmol, 0.1 eq.) was added into a solution of tert-butyl 3-[(trimethylsilyl)ethynyl]-1H-indazole-1-carboxylate (20 g; 63.6 mmol; 1.0 eq.) in EtOH (400 mL) and the reaction mixture was stirred overnight at RT. Solvent was removed under vacuum while maintaining bath temperature below 25° C. The residue was dissolved in Et2O, washed with water (twice) and brine (four times). Organic layer was dried over magnesium sulfate, filtered and concentrated to afford the title compound as a brown solid (7.1 g, 80%). 1H NMR (300 MHz, DMSO-d6) δ: 13.44 (s, 1H), 7.71 (d, J=8.5 Hz, 1H), 7.59 (d; J=8.5 Hz, 1H), 7.41 (m, 1H), 7.22 (m, 1H), 4.50 (s, 1H).

後処理

  1. customSolvent was removed under vacuum
  2. temperaturewhile maintaining bath temperature below 25° C
  3. dissolutionThe residue was dissolved in Et2O
  4. washwashed with water (twice) and brine (four times)
  5. dry with materialOrganic layer was dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-658d6232161e46f58249e9490b24fa8c
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09073892B2

反応ノート

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