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Pyridine → HCID 58734245, 화합물

HRID 2080524
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HRID 2080524 반응식
C(Cl)Cl.[Cl:4][C:5]1[C:6]([CH:12]([S:21]([C:24]2[CH:29]=[CH:28][C:27]([Cl:30])=[CH:26][CH:25]=2)(=[O:23])=[O:22])[C:13]2[CH:18]=[C:17]([F:19])[CH:16]=[CH:15][C:14]=2[F:20])=[CH:7][C:8]([NH2:11])=[N:9][CH:10]=1.N1C=CC=CC=1.Cl[S:38]([CH2:41][C:42]([O:44][CH2:45][CH3:46])=[O:43])(=[O:40])=[O:39]>CCCCCC.C(OCC)(=O)C>[CH2:45]([O:44][C:42](=[O:43])[CH2:41][S:38]([NH:11][C:8]1[CH:7]=[C:6]([CH:12]([S:21]([C:24]2[CH:29]=[CH:28][C:27]([Cl:30])=[CH:26][CH:25]=2)(=[O:23])=[O:22])[C:13]2[CH:18]=[C:17]([F:19])[CH:16]=[CH:15][C:14]=2[F:20])[C:5]([Cl:4])=[CH:10][N:9]=1)(=[O:40])=[O:39])[CH3:46]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 1049Pyridine2회HCID 6344Dichloromethane3회HCID 12225100Ethyl (chlorosulfonyl)acetate2회HCID 23114671[5-Chloro-4-[(4-chlorophenylsulfonyl)(2,5-difluorophenyl)methyl]pyridin-2-yl]amine

생성물 1

HCID 58734245HCID 58734245, 화합물수율 53.4%

시약·촉매·용매 2

HCID 8058
Hexane
용매
HCID 8857Ethyl Acetate용매

실험 절차

To a methylene chloride (10 ml) solution of the [5-chloro-4-[(4-chlorophenylsulfonyl)(2,5-difluorophenyl)methyl]pyridin-2-yl]amine (331 mg, 0.771 mmol) obtained in Example 196 and pyridine (94 μl, 1.16 mmol) was added a methylene chloride (2 ml) solution of ethyl chlorosulfonylacetate (216 mg, 1.16 mmol) at 0° C. After the resulting mixture was stirred at room temperature for 12 hours, pyridine (94 up, 1.16 mmol) and a methylene chloride (2 ml) solution of ethyl chlorosulfonylacetate (216 mg, 1.16 mmol) were added sequentially at 0° C. The resulting mixture was stirred at room temperature for 9 hours and then, the reaction mixture was concentrated under reduced pressure. To the residue thus obtained was added ethyl acetate. The resulting mixture was washed sequentially with a saturated aqueous solution of sodium bicarbonate and brine, 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 (=3:1) eluate was concentrated under reduced pressure to give the title compound (239 mg, 0.412 mmol, 53%) as a white solid.

후처리

  1. stirringThe resulting mixture was stirred at room temperature for 9 hours
  2. concentrationthe reaction mixture was concentrated under reduced pressure
  3. customTo the residue thus obtained
  4. washThe resulting mixture was washed sequentially with a saturated aqueous solution of sodium bicarbonate and brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated under reduced pressure
  8. customThe residue thus obtained
  9. concentrationethyl acetate (=3:1) eluate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-52f9bad9d11948c28528bec9d9323d2a
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07932271B2

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