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Hydrochloric Acid → HCID 58734243, 화합물

HRID 2080527
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HRID 2080527 반응식
C([O:3][C:4](=[O:36])[CH2:5][S:6]([NH:9][C:10]1[CH:15]=[C:14]([CH:16]([S:25]([C:28]2[CH:33]=[CH:32][C:31]([Cl:34])=[CH:30][CH:29]=2)(=[O:27])=[O:26])[C:17]2[CH:22]=[C:21]([F:23])[CH:20]=[CH:19][C:18]=2[F:24])[C:13]([Cl:35])=[CH:12][N:11]=1)(=[O:8])=[O:7])C.O.[OH-].[Li+].Cl.FC(F)(F)C(O)=O>O1CCCC1.O.C(Cl)Cl.CO>[Cl:35][C:13]1[C:14]([CH:16]([S:25]([C:28]2[CH:33]=[CH:32][C:31]([Cl:34])=[CH:30][CH:29]=2)(=[O:27])=[O:26])[C:17]2[CH:22]=[C:21]([F:23])[CH:20]=[CH:19][C:18]=2[F:24])=[CH:15][C:10]([NH:9][S:6]([CH2:5][C:4]([OH:36])=[O:3])(=[O:8])=[O:7])=[N:11][CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 4

HCID 313Hydrochloric AcidHCID 6422Trifluoroacetic acidHCID 168937Lithium hydroxide, monohydrateHCID 58734245HCID 58734245, 화합물

생성물 1

HCID 58734243HCID 58734243, 화합물수율 94.2%

시약·촉매·용매 4

HCID 887Methanol용매
HCID 962Water용매
HCID 6344Dichloromethane용매
HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of the ethyl[[[5-chloro-4-[(4-chlorophenylsulfonyl)(2,5-difluorophenyl)methyl]pyridin-2-yl]amino]sulfonyl]acetate (60 mg, 0.104 mmol) obtained in Example 283 in a mixture of tetrahydrofuran (5 ml) and water (1 ml) was added lithium hydroxide monohydrate (9.1 mg, 0.218 mmol). The resulting mixture was stirred at room temperature for 2 hours. To the reaction mixture was added 1N hydrochloric acid. The resulting mixture was extracted with methylene chloride. The extract was dried over anhydrous sodium sulfate, and filtered. The filtrate was concentrated under reduced pressure. The residue thus obtained was subjected to silica gel column chromatography. The fraction obtained from the methanol:methylene chloride (=1:30) eluate containing 0.5% trifluoroacetic acid was concentrated under reduced pressure to give the title compound (54 mg, 0.098 mmol, 94%) as a white solid.

후처리

  1. extractionThe resulting mixture was extracted with methylene chloride
  2. dry with materialThe extract was dried over anhydrous sodium sulfate
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customThe residue thus obtained
  6. concentrationwas concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-4306c06b66e54fdb8d8cdfaff6fafe9f
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07932271B2

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