Trifluoroacetic acid → 5-Bromo-2-(1-propylpyrrolidin-3-yl)pyrimidine

HRID 1260240ノート

反応式

HRID 1260240 の反応式
CO[CH2:3][N:4]([CH2:11][CH2:12][CH3:13])[CH2:5][CH2:6][Si](C)(C)C.[Br:14][C:15]1[CH:16]=[N:17][C:18]([CH:21]=C)=[N:19][CH:20]=1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[Br:14][C:15]1[CH:16]=[N:17][C:18]([CH:21]2[CH2:6][CH2:5][N:4]([CH2:11][CH2:12][CH3:13])[CH2:3]2)=[N:19][CH:20]=1

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 536286645-Bromo-2-vinylpyrimidineHCID 86761882HCID 86761882、化合物

生成物 1

HCID 574700825-Bromo-2-(1-propylpyrrolidin-3-yl)pyrimidine収率 35.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

実験手順

Methoxymethyl-propyl-trimethylsilanylethyl-amine (14.13 g, 74.61 mmol) in CH2Cl2 (4 ml) was added dropwise to a 0° C. cooled solution of 5-bromo-2-vinyl-pyrimidine (2 g, 10.80 mmol) and TFA (210 μl, 2.72 mmol) in CH2Cl2 (45 ml) over a period of 20 min. The reaction mixture was then stirred at room temperature for 2 h. The crude material was diluted with CH2Cl2, washed with saturated aqueous NaHCO3 and the organic layer was dried over Na2SO4 and evaporated. The residue was chromatographied on silica gel (CH2Cl2:methanol, 97:3) to afford the title compound (1.03 g, 34%) as a brown oil.

後処理

  1. washwashed with saturated aqueous NaHCO3
  2. dry with materialthe organic layer was dried over Na2SO4
  3. customevaporated

出典と根拠

ORDレコード
ord-10acffa648de49b48cec2deafb6a4dcf
出典データセット
uspto-grants-2013_06
特許番号
US08470810B2

反応ノート

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