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

Sodium Hydroxide → HCID 54013597, 화합물

HRID 1277986
노트
인쇄 미리보기

반응식

HRID 1277986 반응식
C([O:3][C:4]([CH:6]1[CH:8]([CH:9]=[C:10]([Br:18])[C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=2)[C:7]1([CH3:20])[CH3:19])=[O:5])C.[OH-].[Na+]>C(O)C.O>[CH3:19][C:7]1([CH3:20])[CH:8]([CH:9]=[C:10]([Br:18])[C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=2)[CH:6]1[C:4]([OH:5])=[O:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 53782350HCID 53782350, 화합물

생성물 1

HCID 54013597HCID 54013597, 화합물수율 81.9%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

50 g (0.14 mol) of 2,2-dimethyl-3-(2-bromo-2-(4-chloro-phenyl)-vinyl)-cyclopropanecarboxylic acid ethyl ester were dissolved in 100 ml of ethanol, a solution of 6 g (0.15 mol) of sodium hydroxide in 100 ml of water was then added and the mixture was heated to the reflux temperature for 4 hours, while stirring. The ethanol was then distilled off under a waterpump vacuum, the residue was taken up in 300 ml of warm water and the mixture was extracted once with 300 ml of methylene chloride. The aqueous phase was separated off, acidified with concentrated hydrochloric acid and then extracted with 2 portions of 300 ml of methylene chloride. The organic phase was then separated off and dried over magnesium sulphate and the solvent was distilled off under a waterpump vacuum. Last residues of solvent were removed by brief incipient distillation under 2 mm Hg at a bath temperature of 60° C. 37.8 g (81.9% of theory) of 2,2-dimethyl-3 -(2-bromo-2-(4-chlorophenyl)-vinyl)-cyclopropanecarboxylic acid (cis and trans, E and Z isomer mixture) were then obtained as a very viscous yellow oil. The structure was confirmed by the 1H-NMR spectrum.

후처리

  1. temperaturethe mixture was heated to the reflux temperature for 4 hours
  2. distillationThe ethanol was then distilled off under a waterpump vacuum
  3. extractionthe mixture was extracted once with 300 ml of methylene chloride
  4. customThe aqueous phase was separated off
  5. extractionextracted with 2 portions of 300 ml of methylene chloride
  6. customThe organic phase was then separated off
  7. dry with materialdried over magnesium sulphate
  8. distillationthe solvent was distilled off under a waterpump vacuum
  9. customLast residues of solvent were removed by brief incipient distillation under 2 mm Hg at a bath temperature of 60° C

출처 및 근거

ORD 기록
ord-acaa38f719f0462696d330c14aff2333
출처 데이터셋
uspto-grants-1981_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04279920

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트