Trifluoroacetic acid → 1-(4-Methyl-1H-pyrazol-1-YL)cyclopropane-1-carboxylic acid

HRID 931063ノート

反応式

HRID 931063 の反応式
[CH3:1][C:2]1[CH:3]=[N:4][N:5]([C:7]2([C:10]([O:12]C(C)(C)C)=[O:11])[CH2:9][CH2:8]2)[CH:6]=1.FC(F)(F)C(O)=O>ClCCl>[CH3:1][C:2]1[CH:3]=[N:4][N:5]([C:7]2([C:10]([OH:12])=[O:11])[CH2:8][CH2:9]2)[CH:6]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acid3 回HCID 117966666tert-butyl 1-(4-methyl-1H-pyrazol-1-yl)cyclopropanecarboxylate

生成物 1

HCID 898536841-(4-Methyl-1H-pyrazol-1-YL)cyclopropane-1-carboxylic acid収率 220.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Into a 100 mL pear shaped flask containing tert-butyl 1-(4-methyl-1H-pyrazol-1-yl)cyclopropanecarboxylate (218 mg, 0.981 mmol) were added dichloromethane (5 mL) and trifluoroacetic acid (0.2 mL, 3 mmol). The clear solution was stirred at room temperature for 30 minutes after which another 0.3 mL of trifluoroacetic acid were added. The mixture was stirred at room temperature for 45 minutes and another 0.3 mL of trifluoroacetic acid were added. The mixture was stirred at room temperature for 18 h. The solvent and excess of trifluoroacetic acid were removed under reduced pressure to afford the title compound (360 mg). The material was used without further purification. 1H NMR (400 MHz, CDCl3) δ 1.78 (m, 2H), 2.02 (m, 2H), 2.17 (s, 3H), 7.54 (s, 1H), 7.74 (s, 1H).

後処理

  1. additionwere added
  2. stirringThe mixture was stirred at room temperature for 18 h
  3. customThe solvent and excess of trifluoroacetic acid were removed under reduced pressure

出典と根拠

ORDレコード
ord-ea61894d7ae84311a5faf5d8d69304b2
出典データセット
uspto-grants-2016_03
特許番号
US09296745B2

反応ノート

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