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Potassium Carbonate → HCID 67326673、化合物

HRID 1500744
ノート
印刷プレビュー

反応式

HRID 1500744 の反応式
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
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 10011938Pyrimidine, 2-ethynyl-4-methoxy- (9CI)HCID 12291499HCID 12291499、化合物

生成物 1

HCID 67326673HCID 67326673、化合物収率 74%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-5ffa381ac93e4e069d49d3fd198ea282
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09206183B2

反応ノート

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