Potassium Carbonate → HCID 44478092, 화합물

HRID 2387710노트

반응식

HRID 2387710 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 44478092HCID 44478092, 화합물수율 60%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-76538b7f26d04baf89807dc939ae0aa2
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08268855B2

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