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Ethanol → 2-Isopropylamino-6-methyl-pyrimidine-4-carboxylic acid ethyl ester

HRID 2069420
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HRID 2069420 반응식
[CH:1]([NH:4][C:5]1[N:10]=[C:9]([C:11]([OH:13])=[O:12])[CH:8]=[C:7]([CH3:14])[N:6]=1)([CH3:3])[CH3:2].[CH2:15](O)[CH3:16]>OS(O)(=O)=O>[CH2:15]([O:12][C:11]([C:9]1[CH:8]=[C:7]([CH3:14])[N:6]=[C:5]([NH:4][CH:1]([CH3:3])[CH3:2])[N:10]=1)=[O:13])[CH3:16]
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참가 물질

4

반응물 2

HCID 702EthanolHCID 669337152-(Isopropylamino)-6-methylpyrimidine-4-carboxylic acid

생성물 1

HCID 685068162-Isopropylamino-6-methyl-pyrimidine-4-carboxylic acid ethyl ester

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

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온도
80 °C

실험 절차

To a solution of 2-isopropylamino-6-methyl-pyrimidine-4-carboxylic acid (1.27 g, 6.53 mmol) in ethanol (20 mL), concentrated H2SO4 (4 mL) is added. The reaction mixture is stirred at 80° C. for 18 h and is then evaporated. The residue is dissolved in EtOAc, washed with sat. aq. NaHCO3 and water, dried over MgSO4, filtered and evaporated. The crude compound is purified by CC on silica gel (eluting with Heptane/EtOAc 4:1) to give 2-isopropylamino-6-methyl-pyrimidine-4-carboxylic acid ethyl ester as a yellow oil (1.46 g); LC-MS: tR=0.97; [M+H]+=224.49.

후처리

  1. customis then evaporated
  2. dissolutionThe residue is dissolved in EtOAc
  3. washwashed with sat. aq. NaHCO3 and water
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customevaporated
  7. customThe crude compound is purified by CC on silica gel (eluting with Heptane/EtOAc 4:1)

출처 및 근거

ORD 기록
ord-6c7da20e7f7d407bbe59875753ee6b89
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08299086B2

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