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

Hydrochloric Acid → 1-(3-Hydroxy-3-methyl-4-pentynyl)-3-methyl-7-propylxanthine

HRID 1738792
노트
인쇄 미리보기

반응식

HRID 1738792 반응식
[CH3:1][N:2]1[C:10]2[N:9]=[CH:8][N:7]([CH2:11][CH2:12][CH3:13])[C:6]=2[C:5](=[O:14])[N:4]([CH2:15][CH2:16]C(=O)C)[C:3]1=[O:20].[C-:21]#[C-:22].[Li+].[Li+].[Cl-].[Ce+3].[Cl-].[Cl-].Cl.[O:30]1[CH2:35][CH2:34]OCC1>C1(C)C=CC=CC=1.O>[OH:30][C:35]([CH3:34])([C:21]#[CH:22])[CH2:16][CH2:15][N:4]1[C:5](=[O:14])[C:6]2[N:7]([CH2:11][CH2:12][CH3:13])[CH:8]=[N:9][C:10]=2[N:2]([CH3:1])[C:3]1=[O:20]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 24636Cerium(III) chlorideHCID 312751,4-Dioxane2회HCID 153909233-Methyl-1-(3-oxobutyl)-7-propylxanthineHCID 178462446HCID 178462446, 화합물

생성물 1

HCID 218393481-(3-Hydroxy-3-methyl-4-pentynyl)-3-methyl-7-propylxanthine

시약·촉매·용매

2
HCID 962Water용매HCID 1140Toluene용매2회

반응 조건

온도
50 °C

실험 절차

A solution of 55.7 g (0.2 mol) of 3-methyl-1-(3-oxobutyl)-7-propylxanthine in a mixture of 200 ml each of dioxane and toluene was added dropwise in 45 minutes to a stirred suspension of 36.8 g (0.4 mol) of lithium acetylide as ethylenediamine complex and 98.6 g (0.4 mol) of anhydrous cerium(III) chloride in a mixture of 500 ml each of dry dioxane and toluene at 50° C. The mixture was then stirred at 50° C. for 7 hours, cooled and, after addition of cold water and acidification with 2 N hydrochloric acid, intensively extracted with chloroform, the extract was washed with water, dried over sodium sulfate and evaporated under reduced pressure, and the residue was purified by filtration through a silica gel column in the eluent chloroform/methanol (50:1), resulting in 35.0 g (58% of theory) of solid, which was recrystallized from ethanol with large losses.

후처리

  1. temperaturecooled
  2. extractionintensively extracted with chloroform
  3. washthe extract was washed with water
  4. dry with materialdried over sodium sulfate
  5. customevaporated under reduced pressure
  6. filtrationthe residue was purified by filtration through a silica gel column in the eluent chloroform/methanol (50:1)
  7. customresulting in 35.0 g (58% of theory) of solid, which
  8. customwas recrystallized from ethanol with large losses

출처 및 근거

ORD 기록
ord-4b4f1570a05048a4987b41ef0679aeb2
출처 데이터셋
uspto-grants-1999_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05965555

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트