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

Water → Ethyl 3-(2-chloro-4-fluoro-5-nitrophenyl)-2-propenoate

HRID 1940483
노트
인쇄 미리보기

반응식

HRID 1940483 반응식
[Cl:1][C:2]1[CH:9]=[C:8]([F:10])[C:7]([N+:11]([O-:13])=[O:12])=[CH:6][C:3]=1[CH:4]=O.[Br-].[C:15]([CH2:20][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)([O:17][CH2:18][CH3:19])=[O:16].C(N(CC)CC)C.O>C1C=CC=CC=1.C(OCC)(=O)C>[Cl:1][C:2]1[CH:9]=[C:8]([F:10])[C:7]([N+:11]([O-:13])=[O:12])=[CH:6][C:3]=1[CH:4]=[CH:20][C:15]([O:17][CH2:18][CH3:19])=[O:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 73731(Ethoxycarbonylmethyl)triphenylphosphonium bromideHCID 135637752-Chloro-4-fluoro-5-nitrobenzaldehyde

생성물 1

HCID 54527423Ethyl 3-(2-chloro-4-fluoro-5-nitrophenyl)-2-propenoate수율 60.1%

시약·촉매·용매 2

HCID 241
Benzene
용매
HCID 8857Ethyl Acetate용매

실험 절차

A stirred mixture of the compound of Step C, Example 2, (11.5 gm, 56.51 mmol), (carbethoxymethyl)triphenylphosphonium bromide (24.2 gm, 56.51 mmol) and triethylamine (50 mL) in benzene (200 mL), under N2, was heated to reflux for 1 hour. Water (200 mL) and ethyl acetate (200 mL) were added. The organic layer was separated, dried over magnesium sulfate and evaporated under reduce pressure to dryness. The residue was chromatographed on silica gel using hexane:EtOAc (15:5) mixture as eluent. The fractions were combined and evaporated under reduce pressure to obtain the title compound of Step D (9.3 gm, 60%) as a yellow solid; m.p. 86°-88° C.,

후처리

  1. temperatureunder N2, was heated
  2. temperatureto reflux for 1 hour
  3. customThe organic layer was separated
  4. dry with materialdried over magnesium sulfate
  5. customevaporated
  6. customThe residue was chromatographed on silica gel
  7. customevaporated

출처 및 근거

ORD 기록
ord-b5c56af113654a1082ea3463ce1d1e0a
출처 데이터셋
uspto-grants-1997_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05700761

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트