Potassium Carbonate → HCID 44478092、化合物

HRID 17107ノート

反応式

HRID 17107 の反応式
C(=O)([O-])[O-].[K+].[K+].C[Si]([C:11]#[C:12][C:13]1[N:18]=[C:17]([NH:19][C:20](=[O:22])[CH3:21])[CH:16]=[CH:15][CH:14]=1)(C)C>CO>[C:12]([C:13]1[N:18]=[C:17]([NH:19][C:20](=[O:22])[CH3:21])[CH:16]=[CH:15][CH:14]=1)#[CH:11]

参加物

4

反応物 2

HCID 11430Potassium CarbonateHCID 44478150N-(6-(2-(Trimethylsilyl)ethynyl)-2-pyridinyl)acetamide

生成物 1

HCID 44478092HCID 44478092、化合物収率 60%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Anhydrous potassium carbonate (110 mg, 0.8 mmoles) was added to a solution of N-(6-((trimethylsilyl)ethynyl)pyridine-2-yl)acetamide (1.86 g, 8 mmol) in 20 ml anhydrous methanol. The reaction mixture was stirred at room temperature for fifteen minutes then filtered. The filtrate was concentrated in vacuo. The crude product mixture was chromatographed on Silica Gel (230-400 Mesh) eluting with 2.5% MeOH/98% CH2Cl2 to yield A436.1 as an off-white solid. (770 mg, 60% yield). M+H+=218.20 1H NMR (400 MHz) MEOD δ 8.13 (m, 1H), 7.75 (m, 1H), 7.27 (m, 1H), 3.65 (s, 1H), 2.18 (s, 3H).

後処理

  1. filtrationthen filtered
  2. concentrationThe filtrate was concentrated in vacuo
  3. customThe crude product mixture was chromatographed on Silica Gel (230-400 Mesh)
  4. washeluting with 2.5% MeOH/98% CH2Cl2
  5. customto yield A436.1 as an off-white solid

出典と根拠

ORDレコード
ord-21d8f692ec4a4409aa8b70bdc10a11a2
出典データセット
uspto-grants-2010_06
特許番号
US07737279B2

反応ノート

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