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

4-Hydroxybenzaldehyde → Methyl 5-(4-hydroxyphenyl)-3-oxo-4-pentenoate

HRID 617669
노트
인쇄 미리보기

반응식

HRID 617669 반응식
[C:1]([O:7][CH3:8])(=[O:6])[CH2:2][C:3]([CH3:5])=[O:4].[OH:9][C:10]1[CH:17]=[CH:16][C:13]([CH:14]=O)=[CH:12][CH:11]=1.C(O)(=O)C.N1CCCCC1>CC1CCCCC1.O>[OH:9][C:10]1[CH:17]=[CH:16][C:13]([CH:14]=[CH:5][C:3](=[O:4])[CH2:2][C:1]([O:7][CH3:8])=[O:6])=[CH:12][CH:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 1264-HydroxybenzaldehydeHCID 176Acetic AcidHCID 7757Methyl acetoacetateHCID 8082Piperidine

생성물 1

HCID 53678662Methyl 5-(4-hydroxyphenyl)-3-oxo-4-pentenoate수율 82%

시약·촉매·용매 2

HCID 962Water용매
HCID 7962
Methylcyclohexane
용매

실험 절차

##STR7## 232 g (2 mol) of methyl acetoacetate, 244 g (2 mol) of 4-hydroxybenzaldehyde, 24 g (0.4 mol) of glacial acetic acid and 6.8 g (0.08 mol) of piperidine were dissolved in 459 ml of methylcyclohexane. The reaction solution was heated to the boil, and the water of reaction was separated off for one hour in a water separator. After the solvent had been decanted, the product was taken up in diethyl ether, filtered off with suction and dried. 362 g (corresponding to a yield of 82%) of methyl 4-hydroxybenzalacetoacetate were obtained. 22 g (0.1 mol) of methyl 4-hydroxybenzalacetoacetate were dissolved in 100 ml of methanol, and 5.6 g (0.1 mol) of KOH in 38 g of methanol were added. Stirring was carried out for 2.5 hours at room temperature, after which the reaction mixture was evaporated down and the remaining residue was dried. 25 g (corresponding to a yield of 97% of the title compound were obtained in the form of a red solid. The purity of the product was >95%.

후처리

  1. temperatureThe reaction solution was heated to the boil
  2. customwas separated off for one hour in a water separator
  3. customAfter the solvent had been decanted
  4. filtrationfiltered off with suction
  5. customdried

출처 및 근거

ORD 기록
ord-3cb19a1ef8264411b709ac6b9256a86b
출처 데이터셋
uspto-grants-1999_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05951841

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트