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2-Chloropyrimidine → 3-(2-Methyl-pyrimidin-5-yl)-10-(pyrimidin-2-ylamino)-decanoic acid ethyl ester

HRID 2120706
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인쇄 미리보기

반응식

HRID 2120706 반응식
[CH2:1]([O:3][C:4](=[O:22])[CH2:5][CH:6]([C:15]1[CH:16]=[N:17][C:18]([CH3:21])=[N:19][CH:20]=1)[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][NH2:14])[CH3:2].Cl[C:24]1[N:29]=[CH:28][CH:27]=[CH:26][N:25]=1.C(N(CC)C(C)C)(C)C>C(O)C>[O-:3][CH2:1][CH3:2].[NH4+:14].[CH2:1]([O:3][C:4](=[O:22])[CH2:5][CH:6]([C:15]1[CH:16]=[N:17][C:18]([CH3:21])=[N:19][CH:20]=1)[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][NH:14][C:24]1[N:29]=[CH:28][CH:27]=[CH:26][N:25]=1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 744042-ChloropyrimidineHCID 81531DiisopropylethylamineHCID 2062248310-Amino-3-(2-methyl-pyrimidin-5-yl)-decanoic acid ethyl ester

생성물 2

HCID 206224843-(2-Methyl-pyrimidin-5-yl)-10-(pyrimidin-2-ylamino)-decanoic acid ethyl ester수율 66.5%HCID 22341770NH4OEt수율 1%

시약·촉매·용매 1

HCID 702
Ethanol
용매

실험 절차

A solution of 24-7 (360 mg, 1.17 mmol), 2-chloropyrimidine (145 mg, 1.26 mmol), and N,N-diisopropylethylamine (456 mg, 3.53 mmol) in ethanol (5 mL) was heated to 65° C. in a sealed tube (4 days). The solvent was removed in vacuo and the residue diluted in aqueous sodium carbonate and extracted with two portions of dichloromethane. The combined organics were washed with brine and dried (Na2SO4). The solvent was removed in vacuo. PCTLC (SiO2, 4mm, 1% NH4OEt; 10% EtOH; 90% CH2Cl2) afforded 24-8 (150 mg). ESLRMS m/e 386 g/mole (M++H, C21H31N5O2=386 g/mole.)

후처리

  1. customThe solvent was removed in vacuo
  2. additionthe residue diluted in aqueous sodium carbonate
  3. extractionextracted with two portions of dichloromethane
  4. washThe combined organics were washed with brine
  5. dry with materialdried (Na2SO4)
  6. customThe solvent was removed in vacuo

출처 및 근거

ORD 기록
ord-1da75e5ec5944093af75001b29f84e1c
출처 데이터셋
uspto-grants-2004_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06693101B2

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