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Tetrahydrofuran → HCID 23114738, 화합물

HRID 2080525
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HRID 2080525 반응식
O1CCCC1.C([O:8][C:9](=O)[CH2:10][S:11]([NH:14][C:15]1[CH:20]=[C:19]([CH:21]([S:30]([C:33]2[CH:38]=[CH:37][C:36]([Cl:39])=[CH:35][CH:34]=2)(=[O:32])=[O:31])[C:22]2[CH:27]=[C:26]([F:28])[CH:25]=[CH:24][C:23]=2[F:29])[C:18]([Cl:40])=[CH:17][N:16]=1)(=[O:13])=[O:12])C.[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl-].[NH4+]>CCCCCC.CCOCC>[Cl:40][C:18]1[C:19]([CH:21]([S:30]([C:33]2[CH:34]=[CH:35][C:36]([Cl:39])=[CH:37][CH:38]=2)(=[O:32])=[O:31])[C:22]2[CH:27]=[C:26]([F:28])[CH:25]=[CH:24][C:23]=2[F:29])=[CH:20][C:15]([NH:14][S:11]([CH2:10][CH2:9][OH:8])(=[O:13])=[O:12])=[N:16][CH:17]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8028TetrahydrofuranHCID 25517Ammonium ChlorideHCID 21226445Aluminium lithium hydrideHCID 58734245HCID 58734245, 화합물

생성물 1

HCID 23114738HCID 23114738, 화합물수율 63%

시약·촉매·용매 2

HCID 3283Diethyl Ether
용매
HCID 8058Hexane용매

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온도
0 °C

실험 절차

To a tetrahydrofuran (5 ml) solution of ethyl[[[5-chloro-4-[(4-chlorophenylsulfonyl)(2,5-difluorophenyl)methyl]pyridin-2-yl]amino]sulfonyl]acetate (67 mg, 0.116 mmol) was added an ether solution (0.18 ml) of 1M lithium aluminum hydride at 0° C. The resulting mixture was stirred at 0° C. After the termination of the reaction was confirmed by TLC, a saturated aqueous solution of ammonium chloride was added to the reaction mixture. The resulting mixture was filtered through Celite. The filtrate was dried over anhydrous sodium sulfate, and filtered. The filtrate was concentrated under reduced pressure. The residue thus obtained was subjected to flash silica gel column chromatography. The fraction obtained from the hexane:ethyl acetate (=2:1) eluate was concentrated under reduced pressure to give the title compound (39 mg, 0.073 mmol, 63%) as a white solid.

후처리

  1. filtrationThe resulting mixture was filtered through Celite
  2. dry with materialThe filtrate was dried over anhydrous sodium sulfate
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customThe residue thus obtained
  6. concentrationethyl acetate (=2:1) eluate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-b5f6d5d6551a4ffea34dfe6f30d76ec9
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07932271B2

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