Pyridine → 2,6-difluoro-N-[4-[(Z)-hydroxyiminomethyl]-5-[3-(trifluoromethyl)phenyl]-1,3-thiazol-2-yl]benzamide

HRID 1255135노트

반응식

HRID 1255135 반응식
[F:1][C:2]1[CH:27]=[CH:26][CH:25]=[C:24]([F:28])[C:3]=1[C:4]([NH:6][C:7]1[S:8][C:9]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([C:20]([F:23])([F:22])[F:21])[CH:15]=2)=[C:10]([CH:12]=O)[N:11]=1)=[O:5].Cl.[NH2:30][OH:31].N1C=CC=CC=1>CCO.C(Cl)Cl>[F:1][C:2]1[CH:27]=[CH:26][CH:25]=[C:24]([F:28])[C:3]=1[C:4]([NH:6][C:7]1[S:8][C:9]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([C:20]([F:23])([F:22])[F:21])[CH:15]=2)=[C:10](/[CH:12]=[N:30]\[OH:31])[N:11]=1)=[O:5]

참가 물질

6

반응물 3

HCID 1049PyridineHCID 443297Hydroxyamine hydrochlorideHCID 24765490HCID 24765490, 화합물

생성물 1

HCID 590045602,6-difluoro-N-[4-[(Z)-hydroxyiminomethyl]-5-[3-(trifluoromethyl)phenyl]-1,3-thiazol-2-yl]benzamide수율 52.1%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 6344Dichloromethane용매

실험 절차

Into a solution of Compound 67 (180 mg, 0.44 mmol) in 3 mL of EtOH was added hydroxylamine hydrochloride (60 mg, 0.9 mmol) and pyridine (0.5 mL). The solution was stirred at room temperature for 2 hours. The reaction was diluted with 20 mL of CH2Cl2, and the solution was washed with 10 mL of water and dried (Na2SO4), filtered and concentrated. The residue was purified on silica (eluted with 5-100% ethyl acetate in hexane) to give Compound 72 (98 mg, 52%) as a white solid.

후처리

  1. washthe solution was washed with 10 mL of water
  2. dry with materialdried (Na2SO4)
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe residue was purified on silica (eluted with 5-100% ethyl acetate in hexane)

출처 및 근거

ORD 기록
ord-3a166eeedc144869abfcb07c838c2f52
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08455658B2

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