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

Diethyl Ether → 1-(Benzyloxycarbonyl)-4-[(4-nitrophenoxy)methyl]piperidine

HRID 1073204
노트
인쇄 미리보기

반응식

HRID 1073204 반응식
[H-].[Na+].[CH2:3]([O:10][C:11]([N:13]1[CH2:18][CH2:17][CH:16]([CH2:19][OH:20])[CH2:15][CH2:14]1)=[O:12])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.F[C:22]1[CH:27]=[CH:26][C:25]([N+:28]([O-:30])=[O:29])=[CH:24][CH:23]=1.CCOCC>O1CCCC1>[CH2:3]([O:10][C:11]([N:13]1[CH2:18][CH2:17][CH:16]([CH2:19][O:20][C:22]2[CH:27]=[CH:26][C:25]([N+:28]([O-:30])=[O:29])=[CH:24][CH:23]=2)[CH2:15][CH2:14]1)=[O:12])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 3283Diethyl EtherHCID 9590p-FluoronitrobenzeneHCID 24758Sodium hydrideHCID 736490Benzyl 4-(hydroxymethyl)piperidine-1-carboxylate

생성물 1

HCID 199924221-(Benzyloxycarbonyl)-4-[(4-nitrophenoxy)methyl]piperidine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran
용매

실험 절차

Sodium hydride (3.36 g of a 50% dispersion in mineral oil) was added portionwise to a stirred solution of the product of part (i) (17.43 g) in dry tetrahydrofuran (200 ml) and the mixture was stirred at room temperature for 1 hour. 4-Fluoronitrobenzene (9.87 g) was added dropwise and the mixture was stirred for a further 18 hours and then evaporated. Water was added to the residue and the mixture was extracted several times with dichloromethane. The combined extracts were washed with water, dried (MgSO4) and evaporated to give an oil which solidified on trituration with ether. The solid was filtered off, washed with a little ether and crystallised from ethyl acetate/hexane to give the product, (13.51 g), m.p. 121°-122°.

후처리

  1. stirringthe mixture was stirred for a further 18 hours
  2. customevaporated
  3. additionWater was added to the residue
  4. extractionthe mixture was extracted several times with dichloromethane
  5. washThe combined extracts were washed with water
  6. dry with materialdried (MgSO4)
  7. customevaporated
  8. customto give an oil which
  9. filtrationThe solid was filtered off
  10. washwashed with a little ether
  11. customcrystallised from ethyl acetate/hexane
  12. customto give the product, (13.51 g), m.p. 121°-122°

출처 및 근거

ORD 기록
ord-8f2f75eecfd74aa59a3e85bf87ba1241
출처 데이터셋
uspto-grants-1990_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04968704

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트