Trifluoroacetic acid → HCID 89720313, 화합물

HRID 623990노트

반응식

HRID 623990 반응식
[CH3:1][O:2][C:3]12[CH2:12][CH:7]3[CH2:8][CH:9]([CH2:11][CH:5]([N:6]3C(OC(C)(C)C)=O)[CH2:4]1)[CH2:10]2.FC(F)(F)C(O)=O>C(Cl)Cl>[CH3:1][O:2][C:3]12[CH2:4][CH:5]3[CH2:11][CH:9]([CH2:8][CH:7]([NH:6]3)[CH2:12]1)[CH2:10]2

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 89720231HCID 89720231, 화합물

생성물 1

HCID 89720313HCID 89720313, 화합물수율 95%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

To a 50 mL RB flask fitted with magnetic stirrer was charged tert-butyl 5-methoxy-2-azatricyclo[3.3.1.13,7]decane-2-carboxylate, Intermediate-17 (0.1 g, 0.037 mmol) in DCM (5 mL). Then reaction mixture was cooled to 0° C. and trifluoroacetic acid (0.22 g, 1.8 mmol) was added and stirred for 4 hours. After completion of the reaction (reaction was monitored by LCMS) reaction mixture was concentrated followed by trituration with mixture of hexane:ether (1:1) to give Intermediate-18 (0.09 g, yield=95%) as an oily mass.

후처리

  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) reaction mixture
  4. concentrationwas concentrated
  5. additionfollowed by trituration with mixture of hexane:ether (1:1)
  6. customto give Intermediate-18 (0.09 g, yield=95%) as an oily mass

출처 및 근거

ORD 기록
ord-546e7b81baf340cabbf0de398f19ba62
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09303016B2

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