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Potassium Carbonate → HCID 67326673, 화합물

HRID 1500744
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HRID 1500744 반응식
CC1C=C(C)C=C(C)C=1S([O-])(=O)=O.[NH2:14][N+:15]1[CH:20]=[CH:19][C:18]([C:21]#[N:22])=[CH:17][CH:16]=1.[C:23]([C:25]1[N:30]=[C:29]([O:31][CH3:32])[CH:28]=[CH:27][N:26]=1)#[CH:24].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH3:32][O:31][C:29]1[CH:28]=[CH:27][N:26]=[C:25]([C:23]2[CH:24]=[N:14][N:15]3[CH:20]=[CH:19][C:18]([C:21]#[N:22])=[CH:17][C:16]=23)[N:30]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 10011938Pyrimidine, 2-ethynyl-4-methoxy- (9CI)HCID 12291499HCID 12291499, 화합물

생성물 1

HCID 67326673HCID 67326673, 화합물수율 74%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1-Amino-4-cyanopyridinium 2,4,6-trimethylbenzenesulfonate (Preparation 2, 12.10 g, 37.88 mmol) was added in portions over 6 hours to a stirred suspension of 2-ethynyl-4-methoxypyrimidine (Preparation 1b, 2.54 g, 18.94 mmol) and potassium carbonate (3.93 g, 28.43 mmol) in anhydrous N,N′-dimethylformamide (47 mL) at 0° C. and the resulting mixture was stirred at ambient temperature for 48 hours. The solvent was evaporated and dichloromethane was added to the residue. The solid formed was filtered and the filtrate evaporated to dryness. The crude product was purified by flash chromatography (4:1 hexanes/ethyl acetate) to give the title compound (3.51 g, 74%) as a solid.

후처리

  1. customThe solvent was evaporated
  2. additiondichloromethane was added to the residue
  3. customThe solid formed
  4. filtrationwas filtered
  5. customthe filtrate evaporated to dryness
  6. customThe crude product was purified by flash chromatography (4:1 hexanes/ethyl acetate)

출처 및 근거

ORD 기록
ord-5ffa381ac93e4e069d49d3fd198ea282
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09206183B2

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