Trifluoroacetic acid → HCID 86708052, 화합물

HRID 1524350노트

반응식

HRID 1524350 반응식
[CH2:1]([O:8][C:9](=[O:61])[N:10]([C@@H:16]([CH2:36][CH2:37][CH:38]([F:60])[CH2:39][NH:40]C(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[CH2:17][O:18][Si:19]([C:32]([CH3:35])([CH3:34])[CH3:33])([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[CH2:11][CH2:12][CH:13]([CH3:15])[CH3:14])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.FC(F)(F)C(O)=O.C([O-])(O)=O.[Na+]>ClC(Cl)C>[CH2:1]([O:8][C:9](=[O:61])[N:10]([C@@H:16]([CH2:36][CH2:37][CH:38]([F:60])[CH2:39][NH2:40])[CH2:17][O:18][Si:19]([C:32]([CH3:35])([CH3:33])[CH3:34])([C:26]1[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=1)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[CH2:11][CH2:12][CH:13]([CH3:15])[CH3:14])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 516892Sodium BicarbonateHCID 86708053HCID 86708053, 화합물

생성물 1

HCID 86708052HCID 86708052, 화합물수율 100%

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

반응 조건

온도
0 °C

실험 절차

To a stirred solution of the material from Step 9 (225 mg, 0.27 mmol) in dichloroethane (1.3 mL) at 0° C. was added trifluoroacetic acid (500 μL, 6.49 mmol). The reaction mixture was stirred at 0° C. for 1 hour, poured into saturated aqueous NaHCO3, and extracted with dichloromethane (2×). The combined organics were dried over MgSO4, filtered and concentrated in vacuo. The residue was purified by flash chromatography on silica gel using EtOAc-hexanes to afford 160 mg of the title compound. LCMS (M+1)=593.

후처리

  1. extractionextracted with dichloromethane (2×)
  2. dry with materialThe combined organics were dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by flash chromatography on silica gel

출처 및 근거

ORD 기록
ord-4a1f14afa2bc48d0b8766888dd078578
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09079834B2

반응 노트

불러오는 중…