Trifluoroacetic acid → HCID 136232554, 화합물

HRID 1047545노트

반응식

HRID 1047545 반응식
C(O)(C(F)(F)F)=O.[NH:8]1[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2[N:10]=[C:9]1[C:17]1[C:25]2[C:20](=[CH:21][CH:22]=[C:23]([NH:26][C:27]([NH:29][CH:30]3[CH2:34][CH2:33][CH2:32][CH2:31]3)=[O:28])[CH:24]=2)[N:19](C2CCCCO2)[N:18]=1>C(Cl)Cl>[NH:10]1[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[N:8]=[C:9]1[C:17]1[C:25]2[C:20](=[CH:21][CH:22]=[C:23]([NH:26][C:27]([NH:29][CH:30]3[CH2:31][CH2:32][CH2:33][CH2:34]3)=[O:28])[CH:24]=2)[NH:19][N:18]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 136352255HCID 136352255, 화합물

생성물 1

HCID 136232554HCID 136232554, 화합물수율 85.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

TFA (0.3 mL, 4.03 mmol) was added to a solution of 1-(3-(1H-benzo[d]imidazol-2-yl)-1-(tetrahydro-2H-pyran-2-yl)-1H-indazol-5-yl)-3-cyclopentylurea (6 mg, 0.013 mmol) in CH2Cl2 (4 mL). The reaction mixture was stirred at room temperature for 24 h, and then the solvent was removed in vacuo. Purification by flash chromatography (6% CH3OH/CH2Cl2) afforded the title compound (4 mg) as an off-white solid. 1H NMR (400 MHz, CD3OD): δ 8.36 (s, 1H), 7.81 (m, 2H), 7.60 (d, 1H, J=8.8 Hz), 7.46 (m, 3H), 4.11 (t, 1H, J=6.4 Hz), 2.00 (m, 2H), 1.75 (m, 2H), 1.65 (m, 2H), 1.51 (m, 2H); ESI-MS [M+H]+: 361.3.

후처리

  1. customthe solvent was removed in vacuo
  2. customPurification by flash chromatography (6% CH3OH/CH2Cl2)

출처 및 근거

ORD 기록
ord-32ebda5d593b45e5a747ec072a9b37e2
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08569511B2

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