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

HRID 484709
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HRID 484709 반응식
[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)CC1C=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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 4

HCID 14798Sodium HydroxideHCID 200263-Chloro-2-butanoneHCID 516892Sodium BicarbonateHCID 178433550HCID 178433550, 화합물

생성물 1

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

시약·촉매·용매 4

HCID 66133
Benzyl triethylammonium chloride
촉매
HCID 180Acetone용매
HCID 962Water용매
HCID 8028Tetrahydrofuran용매

실험 절차

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-triethylbenzenemethanaminium 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 6).

후처리

  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

출처 및 근거

ORD 기록
ord-5cb0fca29584489c9bb947e5d9a7456e
출처 데이터셋
uspto-grants-1985_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04533665

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