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

Dicyclohexylcarbodiimide → 2-(4-Phenoxyphenoxy)ethyl-4,4-difluorobut-3-enoate

HRID 374606
노트
인쇄 미리보기

반응식

HRID 374606 반응식
[F:1][C:2]([F:8])=[CH:3][CH2:4][C:5]([OH:7])=[O:6].N1(C2C=CN=CC=2)CCCC1.[O:20]([C:27]1[CH:36]=[CH:35][C:30]([O:31][CH2:32][CH2:33]O)=[CH:29][CH:28]=1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.C1(N=C=NC2CCCCC2)CCCCC1>C(OCC)C>[O:20]([C:27]1[CH:28]=[CH:29][C:30]([O:31][CH2:32][CH2:33][O:6][C:5](=[O:7])[CH2:4][CH:3]=[C:2]([F:8])[F:1])=[CH:35][CH:36]=1)[C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 10868DicyclohexylcarbodiimideHCID 755674-PyrrolidinopyridineHCID 46767252-(4-Phenoxyphenoxy)ethanolHCID 148558784,4-Difluorobut-3-enoic acid

생성물 1

HCID 189975052-(4-Phenoxyphenoxy)ethyl-4,4-difluorobut-3-enoate

시약·촉매·용매 1

HCID 3283Diethyl Ether
용매

반응 조건

온도
0 °C

실험 절차

A solution of 3.0 g of 4,4-difluorobut-3-enoic acid in 50 ml of diethyl ether is treated with 0.36 g of 4-pyrrolidinopyridine and 5.66 g of 2-(4-phenoxyphenoxy)ethanol, and the mixture is cooled to 0° C. A total of 5.58 g of N,N'-dicyclohexylcarbodiimide are added in portions at a temperature of between 0° C. and +5° C., the ice-cooling is removed, and the reaction mixture is allowed to come to room temperature in the course of 16 hours, with stirring. The N,N'-dicyclohexylurea which has precipitated as a solid is separated off and discarded. The supematant solution is evaporated. The residue obtained is purified by column chromatography on silica gel (eluent: hexane/ethyl acetate, 9:1). This gives pure 2-(4-phenoxyphenoxy)ethyl 4,4-difilorobut-3-enoate in the form of an oil (refractive index nD23 : 1.5315).

후처리

  1. customis removed
  2. customto come to room temperature in the course of 16 hours
  3. customThe N,N'-dicyclohexylurea which has precipitated as a solid
  4. customis separated off
  5. customThe supematant solution is evaporated
  6. customThe residue obtained
  7. customis purified by column chromatography on silica gel (eluent: hexane/ethyl acetate, 9:1)

출처 및 근거

ORD 기록
ord-c4f4c4f747be44b69f6ddf17756f4fb7
출처 데이터셋
uspto-grants-1996_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05481013

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트