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

Water → tert-butyl(R)-1-(2-(2-hydroxyphenyl)-7-methylquinazolin-4-yl)pyrrolidin-3-ylcarbamate

HRID 2406167
노트
인쇄 미리보기

반응식

HRID 2406167 반응식
[C:1]([C@@H]1CCN(N)C1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].[CH2:14]([N:16]([CH2:19][CH3:20])[CH2:17][CH3:18])[CH3:15].ClC1C2[C:26](=[CH:27][C:28]([CH3:32])=[CH:29][CH:30]=2)[N:25]=[C:24]([C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][C:34]=2[OH:39])[N:23]=1.O.C[N:42](C=O)C>C(Cl)Cl>[OH:39][C:34]1[CH:35]=[CH:36][CH:37]=[CH:38][C:33]=1[C:24]1[N:23]=[C:14]([N:16]2[CH2:19][CH2:20][C@@H:18]([NH:42][C:1](=[O:2])[O:3][C:4]([CH3:7])([CH3:6])[CH3:5])[CH2:17]2)[C:15]2[C:26](=[CH:27][C:28]([CH3:32])=[CH:29][CH:30]=2)[N:25]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 962WaterHCID 6228Dimethylformamide2회HCID 8471TriethylamineHCID 66616410(R)-3-Boc-aminopyrrolidineHCID 1361050322-(4-Chloro-7-methylquinazolin-2-yl)-phenol

생성물 1

HCID 136121326tert-butyl(R)-1-(2-(2-hydroxyphenyl)-7-methylquinazolin-4-yl)pyrrolidin-3-ylcarbamate
수율 55%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a cooled (0-5° C.) solution of (3R)-(+)-3-Boc-aminopyrrolidine (12.0 g, 65 mmol) and triethylamine (19 mL, 129 mmol) in DMF (100 mL) was added a solution of 2-(4-chloro-7-methylquinazolin-2-yl)phenol (17.4 g, 64 mmol) in CH2Cl2 (500 mL) and DMF (100 mL). After stirring the mixture for 5 hours at room temperature, water (900 mL) was added. The aqueous layer was extracted with dichloromethane (3×300 mL), and the combined organic layers were washed with saturated aqueous NaCl solution (300 mL), dried over sodium sulfate, filtered, and evaporated to dryness under reduced pressure. The yellow residue (21 g) was treated with 100 mL methanol at room temperature. The solid was collected by filtration and was washed with methanol to yield tert-butyl (R)-1-(2-(2-hydroxyphenyl)-7-methylquinazolin-4-yl)pyrrolidin-3-ylcarbamate (15.1 g, 55%) as a yellow solid.

후처리

  1. extractionThe aqueous layer was extracted with dichloromethane (3×300 mL)
  2. washthe combined organic layers were washed with saturated aqueous NaCl solution (300 mL)
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. customevaporated to dryness under reduced pressure
  6. additionThe yellow residue (21 g) was treated with 100 mL methanol at room temperature
  7. filtrationThe solid was collected by filtration
  8. washwas washed with methanol

출처 및 근거

ORD 기록
ord-b8cbc46faa0a4e42ba152bd4979571d9
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08809353B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트