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Water → HCID 69057074, 화합물

HRID 1437644
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HRID 1437644 반응식
Cl.[CH:2]([C@H:15]1[C@@H:20]([O:21][CH2:22][C:23]2[CH:28]=[C:27]([C:29]([F:32])([F:31])[F:30])[CH:26]=[C:25]([F:33])[CH:24]=2)[CH2:19][CH2:18][NH:17][CH2:16]1)([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[CH3:34][S:35](Cl)(=[O:37])=[O:36].O>C1COCC1.CCN(CC)CC>[CH:2]([C@H:15]1[C@@H:20]([O:21][CH2:22][C:23]2[CH:28]=[C:27]([C:29]([F:32])([F:30])[F:31])[CH:26]=[C:25]([F:33])[CH:24]=2)[CH2:19][CH2:18][N:17]([S:35]([CH3:34])(=[O:37])=[O:36])[CH2:16]1)([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 962WaterHCID 31297Methanesulfonyl chlorideHCID 69059221HCID 69059221, 화합물

생성물 1

HCID 69057074HCID 69057074, 화합물

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8471Triethylamine용매

실험 절차

To a solution of the compound (28.8 mg) obtained in Example 26 in THF (2.0 ml), Et3N (25.1 μl) was added, methylsulfonyl chloride (9.3 μl) was added at 0° C., and the reaction mixture was reacted at room temperature 24 hours. The reaction mixture was poured into water, and then the product was extracted with ethyl acetate. The organic layer was washed with an aqueous 10% citric acid solution and saturated brine, and dried, and the solvent was evaporated under reduced pressure, and then the residue was purified by preparative HPLC to obtain the title compound.

후처리

  1. customthe reaction mixture was reacted at room temperature 24 hours
  2. extractionthe product was extracted with ethyl acetate
  3. washThe organic layer was washed with an aqueous 10% citric acid solution and saturated brine
  4. customdried
  5. customthe solvent was evaporated under reduced pressure
  6. customthe residue was purified by preparative HPLC

출처 및 근거

ORD 기록
ord-2f8305a2e91b420081e6bfde3c05fcaa
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07622487B2

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