Trifluoroacetic acid → HCID 89720591、化合物

HRID 623992ノート

反応式

HRID 623992 の反応式
[CH:1]1([CH2:4][O:5][C:6]23[CH2:15][CH:10]4[CH2:11][CH:12]([CH2:14][CH:8]([N:9]4C(OC(C)(C)C)=O)[CH2:7]2)[CH2:13]3)[CH2:3][CH2:2]1.FC(F)(F)C(O)=O>C(Cl)Cl>[CH:1]1([CH2:4][O:5][C:6]23[CH2:15][CH:10]4[CH2:11][CH:12]([CH2:14][CH:8]([NH:9]4)[CH2:7]2)[CH2:13]3)[CH2:3][CH2:2]1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 89720588HCID 89720588、化合物

生成物 1

HCID 89720591HCID 89720591、化合物収率 95%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

To a 50 mL RB flask fitted with magnetic stirrer was charged tert-butyl 5-(cyclopropylmethoxy)-2-azatricyclo[3.3.1.13,7]decane-2-carboxylate, Intermediate-19 (50 mg, 0.016 mmol) in DCM (5 mL). Then reaction mixture was cooled to 0° C. and trifluoroacetic acid (0.099 g, 0.084 mmol) was added and stirred for 4 hours. After completion of the reaction (reaction was monitored by LCMS) the reaction mixture was concentrated followed by trituration with mixture of hexane:ether (1:1) to give Intermediate-20 (50 mg, yield=95%) as an oily mass.

後処理

  1. customTo a 50 mL RB flask fitted with magnetic stirrer
  2. customThen reaction mixture
  3. customAfter completion of the reaction (reaction was monitored by LCMS) the reaction mixture
  4. concentrationwas concentrated
  5. additionfollowed by trituration with mixture of hexane:ether (1:1)
  6. customto give Intermediate-20 (50 mg, yield=95%) as an oily mass

出典と根拠

ORDレコード
ord-53c872ebcd3040579693ab3ba35c90cd
出典データセット
uspto-grants-2016_04
特許番号
US09303016B2

反応ノート

読み込み中…