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

HRID 2406167
ノート
印刷プレビュー

反応式

HRID 2406167 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 962WaterHCID 6228Dimethylformamide2 回HCID 8471TriethylamineHCID 66616410(R)-3-Boc-aminopyrrolidineHCID 1361050322-(4-Chloro-7-methylquinazolin-2-yl)-phenol

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b8cbc46faa0a4e42ba152bd4979571d9
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08809353B2

反応ノート

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