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

Hydrochloric Acid → Ethyl 4-amino-5-cyano-2-hydroxy-3-methylbenzoate

HRID 1692502
노트
인쇄 미리보기

반응식

HRID 1692502 반응식
[O-:1][CH2:2][CH3:3].[Na+].[Na].C([O:9][C:10](=O)[CH2:11][CH2:12][CH2:13][CH3:14])(=O)C.C(O[CH:19]=[C:20]([C:23]#[N:24])[C:21]#[N:22])C.Cl.C([OH:28])C>>[CH2:2]([O:1][C:10](=[O:9])[C:11]1[CH:19]=[C:20]([C:21]#[N:22])[C:23]([NH2:24])=[C:13]([CH3:14])[C:12]=1[OH:28])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 6

HCID 313Hydrochloric AcidHCID 702EthanolHCID 671522-(Ethoxymethylene)propanedinitrileHCID 2723922Sodium ethoxideHCID 5360545SodiumHCID 21920893Ethylpropionyl acetate

생성물 1

HCID 2775029Ethyl 4-amino-5-cyano-2-hydroxy-3-methylbenzoate
수율 59%

실험 절차

To a solution of sodium ethoxide (1.3 L) (freshly prepared by addition of sodium metal (7.9 g, 0.35 mol) to ethanol (1.3 L)) at 0° C. was added ethylpropionyl acetate (25 g, 0.17 mol) and the solution was stirred at RT for 1 h. To the above solution was added ethoxymethylene malononitrile (21 g, 0.17 mol) at RT and the reaction mixture was refluxed at 80° C. for 2 h. The reaction mixture was cooled, neutralized to pH=7 by addition of 1.5 N HCl and concentrated under vacuum. The obtained residue was diluted with water (100 mL) and filtered. The solid was washed with water and dried under vacuum at 50° C. to give the crude product (27 g). The crude solid was washed with 5% ethyl acetate in pet. ether which gave pure title compound (22.5 g, 59%).

후처리

  1. temperaturethe reaction mixture was refluxed at 80° C. for 2 h
  2. temperatureThe reaction mixture was cooled
  3. concentrationconcentrated under vacuum
  4. additionThe obtained residue was diluted with water (100 mL)
  5. filtrationfiltered
  6. washThe solid was washed with water
  7. customdried under vacuum at 50° C.
  8. customto give the crude product (27 g)
  9. washThe crude solid was washed with 5% ethyl acetate in pet. ether which

출처 및 근거

ORD 기록
ord-0dce303e64104ca2b6e3d9b983ac9208
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08153800B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트