홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Hydrogen chloride-ethyl acetate → N-{(1S)-2-[(6-{6-[(3,3-difluorocyclobutyl)methoxy]-1,3-benzoxazol-2-yl}-5-fluoropyridin-3-yl)oxy]-1-methylethyl}acetamide

HRID 1026349
노트
인쇄 미리보기

반응식

HRID 1026349 반응식
[F:1][C:2]1([F:36])[CH2:5][CH:4]([CH2:6][O:7][C:8]2[CH:35]=[CH:34][C:11]3[N:12]=[C:13]([C:15]4[N:20]=[CH:19][C:18]([O:21][CH2:22][C@@H:23]([NH:25]C(=O)OC(C)(C)C)[CH3:24])=[CH:17][C:16]=4[F:33])[O:14][C:10]=3[CH:9]=2)[CH2:3]1.Cl.[C:38](OCC)(=[O:40])[CH3:39]>C(OCC)(=O)C>[F:36][C:2]1([F:1])[CH2:5][CH:4]([CH2:6][O:7][C:8]2[CH:35]=[CH:34][C:11]3[N:12]=[C:13]([C:15]4[N:20]=[CH:19][C:18]([O:21][CH2:22][C@@H:23]([NH:25][C:38](=[O:40])[CH3:39])[CH3:24])=[CH:17][C:16]=4[F:33])[O:14][C:10]=3[CH:9]=2)[CH2:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 86666323tert-butyl {(1S)-2-[(6-{6-[(3,3-difluorocyclobutyl)methoxy]-1,3-benzoxazol-2-yl}-5-fluoropyridin-3-yl)oxy]-1-methylethyl}carbamate

생성물 1

HCID 67778439N-{(1S)-2-[(6-{6-[(3,3-difluorocyclobutyl)methoxy]-1,3-benzoxazol-2-yl}-5-fluoropyridin-3-yl)oxy]-1-methylethyl}acetamide

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A mixture of tert-butyl {(1S)-2-[(6-{6-[(3,3-difluorocyclobutyl)methoxy]-1,3-benzoxazol-2-yl}-5-fluoropyridin-3-yl)oxy]-1-methylethyl}carbamate (390 mg), 4 M hydrogen chloride/ethyl acetate (3 mL), and ethyl acetate (3 mL) was stirred at room temperature for 4 hr. The mixture was concentrated under reduced pressure. The residue was mixed with pyridine (3 mL) and acetic anhydride (1 mL). The mixture was stirred at room temperature for 3 days. 1 M hydrochloric acid was added, and the mixture was extracted with ethyl is acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate/methanol) and recrystallization (ethyl acetate) to give the title compound (218 mg) as white crystals.

후처리

  1. concentrationThe mixture was concentrated under reduced pressure
  2. additionThe residue was mixed with pyridine (3 mL) and acetic anhydride (1 mL)
  3. stirringThe mixture was stirred at room temperature for 3 days
  4. addition1 M hydrochloric acid was added
  5. extractionthe mixture was extracted with ethyl
  6. washThe organic layer was washed with brine
  7. dry with materialdried over anhydrous magnesium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate/methanol) and recrystallization (ethyl acetate)

출처 및 근거

ORD 기록
ord-34f7a937fdd8415a8a2400baede4621d
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08729102B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트