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

Pyridine → N-(t-butyldimethylsilyl)-4-(3-benzyloxycarbonyl-2-oxopropyl)-azetidin-2-one

HRID 1493467
노트
인쇄 미리보기

반응식

HRID 1493467 반응식
N1C=CC=CC=1.[Si:7]([N:14]1[CH:17]([CH2:18][CH:19]([OH:31])[CH2:20][C:21]([O:23][CH2:24][C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)=[O:22])[CH2:16][C:15]1=[O:32])([C:10]([CH3:13])([CH3:12])[CH3:11])([CH3:9])[CH3:8]>C(Cl)Cl.[O-2].[O-2].[O-2].[Cr+6]>[Si:7]([N:14]1[CH:17]([CH2:18][C:19](=[O:31])[CH2:20][C:21]([O:23][CH2:24][C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)=[O:22])[CH2:16][C:15]1=[O:32])([C:10]([CH3:13])([CH3:12])[CH3:11])([CH3:9])[CH3:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 1049PyridineHCID 12804719N-(t-butyldimethylsilyl)-4-(3-benzyloxycarbonyl-2-hydroxypropyl)-azetidin-2-one

생성물 1

HCID 12804720N-(t-butyldimethylsilyl)-4-(3-benzyloxycarbonyl-2-oxopropyl)-azetidin-2-one수율 73.2%

시약·촉매·용매 2

HCID 10219390chromium (VI) trioxide촉매HCID 6344Dichloromethane용매2회

실험 절차

Anhydrous CrO3 (2.274 g, 22.74 mmol) is added to a solution of anhydrous pyridine (3.597 g, 45.48 mmol) in anhydrous CH2Cl2 (60 ml). After stirring at room temperature for 15 mins, the reaction mixture is treated all at once with a solution of N-(t-butyldimethylsilyl)-4-(3-benzyloxycarbonyl-2-hydroxypropyl)-azetidin-2-one (1.432 g, 3.79 mmol) in anhydrous CH2Cl2 (25 ml). The resulting mixture is stirred at 25° C. for 5 mins. The CH2Cl2 layer is decanted from the dark, gummy residue which is triturated with more CH2Cl2. The combined CH2Cl2 phase is evaporated i.v. The residue is triturated with diethylether (Et2O) (100 ml) in several portions and the Et2O extracts are filtered to remove chromium salts. The ethereal filtrate is washed with 5% NaHCO3, 1N HCl, 5% NaHCO3 and brine, dried with MgSO4, filtered, and evaporated i.v. to yield N-(t-butyldimethylsilyl)-4-(3-benzyloxycarbonyl-2-oxopropyl)-azetidin-2-one (1.042 g) as a pale yellow oil: ir (neat) 5.72 (3 poorly resolved peaks), 7.59 7.98, 8.42, and 11.93 cm-1 ; nmr (CDCl3) δ0.18 (s,3), 0.22 (s,3), 0.97 (s,9), 2.53 (dd,1), 2.63 (dd,1), 3.13 (dd,1), 3.28 (dd,1), 3.47 (s,2), 3.88 (m,1), 5.17 (s,2), and 7.33 (s,5); mass spectrum m/e 360, 318, and 2.76.

후처리

  1. stirringThe resulting mixture is stirred at 25° C. for 5 mins
  2. customThe CH2Cl2 layer is decanted from the dark, gummy residue which
  3. customis triturated with more CH2Cl2
  4. customThe combined CH2Cl2 phase is evaporated i.v
  5. customThe residue is triturated with diethylether (Et2O) (100 ml) in several portions
  6. filtrationthe Et2O extracts are filtered
  7. customto remove chromium salts
  8. washThe ethereal filtrate is washed with 5% NaHCO3, 1N HCl, 5% NaHCO3 and brine
  9. dry with materialdried with MgSO4
  10. filtrationfiltered
  11. customevaporated i.v

출처 및 근거

ORD 기록
ord-5d961017ea3a4b5ba8c81ce97dc28068
출처 데이터셋
uspto-grants-1991_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05021566

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트