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

Triphenylphosphine → 4-Chloro-7-methoxy-6-[(1-methylpyrrolidin-3-yl)oxy]quinazoline

HRID 640018
노트
인쇄 미리보기

반응식

HRID 640018 반응식
N(C(OCC)=O)=NC(OCC)=O.[Cl:13][C:14]1[C:23]2[C:18](=[CH:19][C:20]([O:25][CH3:26])=[C:21]([OH:24])[CH:22]=2)[N:17]=[CH:16][N:15]=1.[CH3:27][N:28]1[CH2:32][CH2:31][CH:30](O)[CH2:29]1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>ClCCl.CO.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[Cl:13][C:14]1[C:23]2[C:18](=[CH:19][C:20]([O:25][CH3:26])=[C:21]([O:24][CH:30]3[CH2:31][CH2:32][N:28]([CH3:27])[CH2:29]3)[CH:22]=2)[N:17]=[CH:16][N:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 11776TriphenylphosphineHCID 930741-Methyl-3-pyrrolidinolHCID 220568ethyl N-ethoxycarbonyliminocarbamate2회HCID 231324754-Chloro-7-methoxyquinazolin-6-ol

생성물 1

HCID 866093914-Chloro-7-methoxy-6-[(1-methylpyrrolidin-3-yl)oxy]quinazoline수율 29.6%

시약·촉매·용매 3

HCID 11776
Triphenylphosphine
촉매
HCID 887Methanol용매
HCID 6344Dichloromethane용매2회

실험 절차

Diethyl azodicarboxylate (793 mg, 4.56 mmol) was added portionwise at room temperature to a stirred suspension of 4-chloro-7-methoxyquinazolin-6-ol (800 mg, 3.80 mmol), 1-methylpyrrolidin-3-ol (422 mg, 4.18 mmol) and triphenylphosphine (1.3 g, 4.96 mmol) in dichloromethane (16 ml). The reaction mixture was stirred for 1 hour and then a further portion of diethyl azodicarboxylate (360 ul) and triphenylphosphine (0.65 mg) were added. The mixture was stirred for 1 hour and the resulting orange solution was purified directly by silica gel chromatography eluting with a 0-10% mixture of methanol in dichloromethane to 4-chloro-7-methoxy-6-[(1-methylpyrrolidin-3-yl)oxy]quinazoline (330 mg, 28% yield) as a tan coloured solid:

후처리

  1. stirringThe mixture was stirred for 1 hour
  2. customthe resulting orange solution was purified directly by silica gel chromatography

출처 및 근거

ORD 기록
ord-56ccd2ff96864494bc9f73900838ecbb
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07691867B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트