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

HRID 2120706
ノート
印刷プレビュー

反応式

HRID 2120706 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 2

HCID 206224843-(2-Methyl-pyrimidin-5-yl)-10-(pyrimidin-2-ylamino)-decanoic acid ethyl ester収率 66.5%HCID 22341770NH4OEt収率 1%

試薬・触媒・溶媒 1

HCID 702
Ethanol
溶媒

実験手順

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.)

後処理

  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

出典と根拠

ORDレコード
ord-1da75e5ec5944093af75001b29f84e1c
出典データセット
uspto-grants-2004_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06693101B2

反応ノート

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