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

Phosphorus oxychloride → N-(4,6-Dichloropyrido[3,2-d]pyrimidin-2-yl)acetamide

HRID 1517456
노트
인쇄 미리보기

반응식

HRID 1517456 반응식
[C:1]([NH:4][C:5]1[NH:6][C:7](=O)[C:8]2[N:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:9]=2[N:10]=1)(=[O:3])[CH3:2].CCN(C(C)C)C(C)C.O=P(Cl)(Cl)[Cl:28]>O1CCOCC1>[Cl:28][C:7]1[C:8]2[N:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:9]=2[N:10]=[C:5]([NH:4][C:1](=[O:3])[CH3:2])[N:6]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24813Phosphorus oxychlorideHCID 81531DiisopropylethylamineHCID 135978119N-(6-Chloro-4-oxo-1,4-dihydropyrido[3,2-d]pyrimidin-2-yl)acetamide

생성물 1

HCID 57698319N-(4,6-Dichloropyrido[3,2-d]pyrimidin-2-yl)acetamide수율 78.2%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
80 °C

실험 절차

To a suspension of 2-acetamido-6-chloro-3H-pyrido[3,2-d]pyrimidin-4-one (2.38 g, 10 mmol) and DIEA (5.2 mL, 30 mmol) in dioxane (120 mL) was added POCl3 (2.8 mL, 30 mmol). The mixture was heated to 80° C. for 2 hours. After removal of solvent, the residue was stirred with crashed ice for 10 minutes, then extracted with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate and concentrated to dryness providing the pure title compound as a brown solid (2.01 g, yield 78%) which was characterised as follows: MS (m/z) 256.9 [M+H]+.

후처리

  1. customAfter removal of solvent
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated to dryness

출처 및 근거

ORD 기록
ord-13e4a5b4b4e94391ab8561517cdf9ee0
출처 데이터셋
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08232278B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트