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

Aluminium lithium hydride → 2-[(3,5-Bis[1,1-dimethylethyl]-4-hydroxyphenyl)amino]benzaldehyde

HRID 1885231
노트
인쇄 미리보기

반응식

HRID 1885231 반응식
C[O:2][C:3](=O)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[NH:10][C:11]1[CH:16]=[C:15]([C:17]([CH3:20])([CH3:19])[CH3:18])[C:14]([OH:21])=[C:13]([C:22]([CH3:25])([CH3:24])[CH3:23])[CH:12]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cr](Cl)([O-])(=O)=O.[NH+]1C=CC=CC=1>C(OCC)C.C(Cl)Cl>[CH3:25][C:22]([C:13]1[CH:12]=[C:11]([NH:10][C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[CH:3]=[O:2])[CH:16]=[C:15]([C:17]([CH3:18])([CH3:19])[CH3:20])[C:14]=1[OH:21])([CH3:23])[CH3:24]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 21226445Aluminium lithium hydrideHCID 53640968HCID 53640968, 화합물HCID 178418287HCID 178418287, 화합물

생성물 1

HCID 198803512-[(3,5-Bis[1,1-dimethylethyl]-4-hydroxyphenyl)amino]benzaldehyde수율 100%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매2회
HCID 6344
Dichloromethane
용매

실험 절차

2-[(3,5-Bis[1,1 -dimethylethyl]-4-hydroxyphenyl)amino]-benzoic acid methyl ester (1.1 g, 3.1 mmols) is dissolved in 100 mL of diethyl, ether and added to a suspension of lithium aluminum hydride (0.46 g, 12.4 mmols) in 20 mL of diethyl ether at room temperature under an argon atmosphere. After 30 minutes the reaction is quenched with 0.46 mL of water, followed by 0.46 mL of 15% (w/v) aqueous sodium hydroxide and then 1.38 mL of water. The solids are removed by filtration of the reaction mixture into a flask containing sodium dithionite (15 g) and 300 mL of 50% aqueous tetrahydrofuran. The filtrate is concentrated in vacuo and the organics are extracted into two 100 mL portions of methylene chloride. The methylene chloride extracts are washed with 100 mL of brine, dried over magnesium sulfate, and filtered. The filtrate is added to a suspension of pyridinium chlorochromate (2.0 g, 9.3 mmols) and alumina (7.0 g) in 100 mL of methylene chloride. The reaction is stirred at room temperature for 12 hours, then filtered through a silica gel pad which is washed with 100 mL of diethyl ether. The filtrate is concentrated in vacuo and the residue is taken up in 100 mL of tetrahydrofuran. Sodium dithionite (15 g) is dissolved in 100 mL of water and added to the tetrahydrofuran solution. After 15 minutes the mixture is concentrated in vacuo and then extracted with three 50 mL portions of diethyl ether. The ether extract is washed with 50 mL of brine and dried over magnesium sulfate. Evaporation gives 1.0 g (100%) of 2-[(3,5-bis[1,1-dimethylethyl]-4-hydroxyphenyl)amino]benzaldehyde, mp 105°-107° C. An analytical sample is obtained by recrystallization from water/methanol.

후처리

  1. customAfter 30 minutes the reaction is quenched with 0.46 mL of water
  2. customThe solids are removed by filtration of the reaction mixture into a flask
  3. additioncontaining sodium dithionite (15 g) and 300 mL of 50% aqueous tetrahydrofuran
  4. concentrationThe filtrate is concentrated in vacuo
  5. extractionthe organics are extracted into two 100 mL portions of methylene chloride
  6. washThe methylene chloride extracts are washed with 100 mL of brine
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltered
  9. filtrationfiltered through a silica gel pad which
  10. washis washed with 100 mL of diethyl ether
  11. concentrationThe filtrate is concentrated in vacuo
  12. dissolutionSodium dithionite (15 g) is dissolved in 100 mL of water
  13. additionadded to the tetrahydrofuran solution
  14. concentrationAfter 15 minutes the mixture is concentrated in vacuo
  15. extractionextracted with three 50 mL portions of diethyl ether
  16. extractionThe ether extract
  17. washis washed with 50 mL of brine
  18. dry with materialdried over magnesium sulfate
  19. customEvaporation

출처 및 근거

ORD 기록
ord-55555552cbbb4d12b61f811000a69a99
출처 데이터셋
uspto-grants-1992_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05143929

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트