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Sodium Hydroxide → 5-(2-hydroxyethyl)-6-methyl-2-[(1-methyl-2-oxopropyl)thio]-4(3H)-pyrimidinone

HRID 325914
ノート
印刷プレビュー

反応式

HRID 325914 の反応式
[OH:1][C:2]1[C:7]([CH2:8][CH2:9][OH:10])=[C:6]([CH3:11])[N:5]=[C:4]([SH:12])[N:3]=1.[OH-].[Na+].C(=O)([O-])O.[Na+].Cl[CH:21]([CH3:25])[C:22](=[O:24])[CH3:23].[Cl-].C([N+](CC)(CC)CCC1C=CC=CC=1)C>O.O1CCCC1.CC(=O)C>[OH:10][CH2:9][CH2:8][C:7]1[C:2](=[O:1])[NH:3][C:4]([S:12][CH:21]([CH3:25])[C:22](=[O:24])[CH3:23])=[N:5][C:6]=1[CH3:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 14798Sodium HydroxideHCID 200263-Chloro-2-butanoneHCID 516892Sodium BicarbonateHCID 20262408N,N,N-triethylbenzeneethanaminium chlorideHCID 178433550HCID 178433550、化合物

生成物 1

HCID 1356746505-(2-hydroxyethyl)-6-methyl-2-[(1-methyl-2-oxopropyl)thio]-4(3H)-pyrimidinone

試薬・触媒・溶媒

3
HCID 180Acetone溶媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 30 parts of 4-hydroxy-2-mercapto-6-methyl-5-pyrimidineethanol, 6.8 parts of sodium hydroxide, 15 parts of sodium hydrogen carbonate and 100 parts of 2-propanone was stirred at room temperature and there were added 180 parts of tetrahydrofuran and 170 parts of water. Then there were added at once 25 parts of 3-chloro-2-butanone and 0.2 parts of N,N,N-triethylbenzeneethanaminium chloride and the whole was stirred and heated for 1 hour at 60° C. Stirring was continued overnight at room temperature. The reaction mixture was filtered and the filtrate was salted out. The organic phase was separated, dried, filtered and evaporated, yielding 36 parts of 5-(2-hydroxyethyl)-6-methyl-2-[(1-methyl-2-oxopropyl)thio]-4(3H)-pyrimidinone as an oily residue (intermediate 7).

後処理

  1. stirringthe whole was stirred
  2. temperatureheated for 1 hour at 60° C
  3. stirringStirring
  4. filtrationThe reaction mixture was filtered
  5. customThe organic phase was separated
  6. customdried
  7. filtrationfiltered
  8. customevaporated

出典と根拠

ORDレコード
ord-6e4ecfd2bff14e5cb9b1b0c73aa99639
出典データセット
uspto-grants-1984_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04443451

反応ノート

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