Trifluoroacetic acid → (S)-5-((3,4-Dimethoxyphenoxy)methyl)-1-methyl-3-(pyrrolidin-2-yl)-1H-pyrazole

HRID 710052ノート

反応式

HRID 710052 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:26]=[CH:27][C:28]=1[O:29][CH3:30])[O:6][CH2:7][C:8]1[N:12]([CH3:13])[N:11]=[C:10]([C@@H:14]2[CH2:18][CH2:17][CH2:16][N:15]2C(OC(C)(C)C)=O)[CH:9]=1.C(O)(C(F)(F)F)=O>C(Cl)(Cl)Cl>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:26]=[CH:27][C:28]=1[O:29][CH3:30])[O:6][CH2:7][C:8]1[N:12]([CH3:13])[N:11]=[C:10]([C@@H:14]2[CH2:18][CH2:17][CH2:16][NH:15]2)[CH:9]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 86706764(S)-t-Butyl 2-(5-((3,4-dimethoxyphenoxy)methyl)-1-methyl-1H-pyrazol-3-yl)pyrrolidine-1-carboxylate

生成物 1

HCID 86706765(S)-5-((3,4-Dimethoxyphenoxy)methyl)-1-methyl-3-(pyrrolidin-2-yl)-1H-pyrazole収率 102%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To a CHCl3 (1.0 mL) solution of the compound (365 mg) obtained in Example 13-(2), TFA (5.0 mL) was added at 0° C. and the mixture was stirred at room temperature for 2 hours. After concentrating the reaction mixture, saturated aqueous sodium bicarbonate (50 mL) was added and the organic layer extracted with CHCl3 (50 mL×2) was dried (Na2SO4), filtered and concentrated to give the titled compound (283 mg, pale brown oil.)

後処理

  1. concentrationAfter concentrating the reaction mixture, saturated aqueous sodium bicarbonate (50 mL)
  2. additionwas added
  3. extractionthe organic layer extracted with CHCl3 (50 mL×2)
  4. dry with materialwas dried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-c2f5bbf9c3234ffd97451368cc61d6e9
出典データセット
uspto-grants-2015_11
特許番号
US09181229B2

反応ノート

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