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Trifluoroacetic acid → HCID 86687713, 화합물

HRID 1473641
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HRID 1473641 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:6]=[CH:5][C:4]=1[C:13]1[C:22]2[C:17](=[CH:18][C:19]([S:23]([N:26](CC3C=CC(OC)=CC=3)[C:27]3[N:28]=[CH:29][S:30][CH:31]=3)(=[O:25])=[O:24])=[CH:20][CH:21]=2)[CH:16]=[CH:15][N:14]=1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([C:9]([F:10])([F:11])[F:12])[CH:6]=[CH:5][C:4]=1[C:13]1[C:22]2[C:17](=[CH:18][C:19]([S:23]([NH:26][C:27]3[N:28]=[CH:29][S:30][CH:31]=3)(=[O:25])=[O:24])=[CH:20][CH:21]=2)[CH:16]=[CH:15][N:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 86687712HCID 86687712, 화합물

생성물 1

HCID 86687713HCID 86687713, 화합물수율 43%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 1-(2-methoxy-4-(trifluoromethyl)phenyl)-N-(4-methoxybenzyl)-N-(thiazol-4-yl)isoquinoline-6-sulfonamide (0.070 g, 0.120 mmol) in DCM (1.195 ml) was added TFA (0.276 ml, 3.59 mmol) at room temperature. The resulting mixture stirred for a total of 3 weeks, monitoring every few days by LCMS. The crude mixture was concentrated by allowing the DCM to evaporate and taken up in DMSO. The DMSO solution was injected directly onto the Gilson HPLC for purification to provide 24 mgs (43% yield) of desired product. m/z (ESI) 465.9 (M+H)+.

후처리

  1. waitmonitoring every few days by LCMS
  2. concentrationThe crude mixture was concentrated
  3. customto evaporate
  4. customThe DMSO solution was injected directly onto the Gilson HPLC for purification

출처 및 근거

ORD 기록
ord-1dcda931d92c44c1a1af4b208019e75b
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09012443B2

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