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

Sodium Sulfate → 6-Dimethylaminomethyl-2-hydroxymethylpyridine

HRID 1980733
노트
인쇄 미리보기

반응식

HRID 1980733 반응식
[CH3:1][N:2]([CH3:15])[C:3]([C:5]1[N:10]=[C:9]([C:11](OC)=[O:12])[CH:8]=[CH:7][CH:6]=1)=O.[H-].[Al+3].[Li+].[H-].[H-].[H-].[O-]S([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[CH3:15][N:2]([CH2:3][C:5]1[N:10]=[C:9]([CH2:11][OH:12])[CH:8]=[CH:7][CH:6]=1)[CH3:1]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24436Sodium SulfateHCID 13102909Methyl 6-[(dimethylamino)carbonyl]-2-pyridinecarboxylateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 155923006-Dimethylaminomethyl-2-hydroxymethylpyridine수율 32.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 6-(N,N-dimethylcarbamyl-2-carbomethoxypyridine (20.3 g; 97.5 mmoles) [prepared in Step A] in 200 ml of tetrahydrofuran was added to a suspension of lithium aluminum hydride (9.6 g; 0.25 moles) in 500 ml of tetrahydrofuran. The mixture was stirred and heated at reflux temperature under a nitrogen atmosphere for 3 hours then left at ambient temperature overnight. The mixture was decomposed with a saturated aqueous solution of Na2SO4, filtered, dried and evaporated under reduced pressure. The residue was placed on 275 g of aluminum oxide and eluted with methylene chloride. The appropriate fractions were combined and evaporated to give 5.2 g of the title compound.

후처리

  1. temperatureheated
  2. temperatureat reflux temperature under a nitrogen atmosphere for 3 hours
  3. filtrationfiltered
  4. customdried
  5. customevaporated under reduced pressure
  6. washeluted with methylene chloride
  7. customevaporated

출처 및 근거

ORD 기록
ord-5e1b760c1337447887cded273bcc0870
출처 데이터셋
uspto-grants-1985_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04510309

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트