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

Phosphorus oxychloride → ethyl 4-(4-chloro-5H-pyrrolo[3,2-d]pyrimidin-6-yl)benzoate hydrochloride

HRID 1786939
노트
인쇄 미리보기

반응식

HRID 1786939 반응식
O=[C:2]1[NH:7][CH:6]=[N:5][C:4]2[CH:8]=[C:9]([C:11]3[CH:21]=[CH:20][C:14]([C:15]([O:17][CH2:18][CH3:19])=[O:16])=[CH:13][CH:12]=3)[NH:10][C:3]1=2.P(Cl)(Cl)([Cl:24])=O>O1CCOCC1>[ClH:24].[Cl:24][C:2]1[C:3]2[NH:10][C:9]([C:11]3[CH:21]=[CH:20][C:14]([C:15]([O:17][CH2:18][CH3:19])=[O:16])=[CH:13][CH:12]=3)=[CH:8][C:4]=2[N:5]=[CH:6][N:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 136354574ethyl 4-(4-oxo-4,5-dihydro-3H-pyrrolo[3,2-d]pyrimidin-6-yl)benzoate

생성물 1

HCID 86615760ethyl 4-(4-chloro-5H-pyrrolo[3,2-d]pyrimidin-6-yl)benzoate hydrochloride수율 94.2%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
110 °C

실험 절차

A mixture of ethyl 4-(4-oxo-4,5-dihydro-3H-pyrrolo[3,2-d]pyrimidin-6-yl)benzoate (2.97 g) and phosphoryl chloride (16.45 g) was stirred at 110° C. for 1 hr, dioxane (10 mL) was added and the mixture was heated under reflux for 4 hrs. After concentration under reduced pressure, ethanol (30 mL) was added to the residue and, after stirring at room temperature for 30 min, the precipitated solid was collected by filtration. The solid washed with ethanol and dried under reduced pressure at 60° C. to give the title compound (3.34 g).

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 4 hrs
  3. concentrationAfter concentration under reduced pressure, ethanol (30 mL)
  4. additionwas added to the residue
  5. stirringafter stirring at room temperature for 30 min
  6. filtrationthe precipitated solid was collected by filtration
  7. washThe solid washed with ethanol
  8. customdried under reduced pressure at 60° C.

출처 및 근거

ORD 기록
ord-f73f8bea7c904e2399764dcdefce25f6
출처 데이터셋
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07507740B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트