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

Hydrochloric Acid → 4-Acetyl-2-methylbenzoic acid

HRID 1848280
노트
인쇄 미리보기

반응식

HRID 1848280 반응식
C(=O)([O-])[O-].[K+].[K+].[CH:7]([O:9]CCCC)=[CH2:8].C1(P(C2C=CC=CC=2)CCCP(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.Br[C:44]1[CH:52]=[CH:51][C:47]([C:48]([OH:50])=[O:49])=[C:46]([CH3:53])[CH:45]=1.Cl>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C(O)CCC>[C:7]([C:44]1[CH:52]=[CH:51][C:47]([C:48]([OH:50])=[O:49])=[C:46]([CH3:53])[CH:45]=1)(=[O:9])[CH3:8]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 8108Butyl vinyl etherHCID 11430Potassium CarbonateHCID 812191,3-Bis(diphenylphosphino)propaneHCID 995704-Bromo-2-methylbenzoic acid

생성물 1

HCID 534355544-Acetyl-2-methylbenzoic acid수율 95%

시약·촉매·용매 2

HCID 167845palladium(II) acetate촉매HCID 2631-Butanol용매

반응 조건

온도
80 °C

실험 절차

16.6 g (120 mmol) of potassium carbonate, 30.1 g (300 mmol) of n-butyl vinyl ether, 44.9 mg (0.2 mmol) of palladium acetate and 0.247 g (0.6 mmol) of 1,3-bis(diphenylphosphino)propane were added to a suspension solution of 21.5 g (100 mmol) of 4-bromo-2-methylbenzoic acid and 64.5 g of n-butanol. After degassing and nitrogen-purging inside of the reactor, the mixture was refluxed for 5 hours. After cooling the reaction solution to 80° C., n-butanol and n-butyl vinyl ether were distilled off under reduced pressure. After adding 172 g of toluene and 108 g of water, the mixture was neutralized by adding 15.6 g (150 mmol) of concentrated hydrochloric acid, and the water phase was separated. The obtained toluene solution was analyzed by a quantitative analysis method using HPLC. A content of 4-acetyl-2-methylbenzoic acid was 16.9 g (yield 95%).

후처리

  1. customAfter degassing
  2. customnitrogen-purging inside of the reactor
  3. temperaturethe mixture was refluxed for 5 hours
  4. distillationn-butanol and n-butyl vinyl ether were distilled off under reduced pressure
  5. additionAfter adding 172 g of toluene and 108 g of water
  6. customthe water phase was separated

출처 및 근거

ORD 기록
ord-dfe81019fdd04925934a5b580050f4b2
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08952175B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트