Propyl mercaptan → HCID 86658684, 화합물

HRID 42695

반응식

HRID 42695 반응식
[CH2:1]([SH:4])[CH2:2][CH3:3].[H-].[Na+].Cl[C:8]1[N:13]([CH3:14])[C:12](=[O:15])[N:11]([CH3:16])[C:10](=[O:17])[C:9]=1[CH:18]=[O:19]>O1CCOCC1>[CH3:14][N:13]1[C:8]([S:4][CH2:1][CH2:2][CH3:3])=[C:9]([CH:18]=[O:19])[C:10](=[O:17])[N:11]([CH3:16])[C:12]1=[O:15]

참가 물질

5

반응물 3

HCID 7848Propyl mercaptanHCID 24758Sodium hydrideHCID 3199716-Chloro-5-formyl-1,3-dimethyluracil

생성물 1

HCID 86658684HCID 86658684, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

To a stirred solution of propane-1-thiol (2.30 mmol) in dry 1,4-dioxane (4 ml), NaH (2.30 mmol) was added under argon. To the mixture, a solution of 6-chloro-1,3-dimethyl-2,4-dioxo-1,2,3,4-tetrahydropyrimidine-5-carbaldehyde (2 mmol) in dry 1,4-dioxane (8 ml) was added at 5-8° C. in one portion. The mixture was stirred at room temperature until the starting material was consumed (monitored by TLC). Then the mixture was poured onto ice water (50 ml) and the aqueous phase was extracted with ethyl acetate (3×30 ml). The combined organic phases were washed with water and dried over anhydrous MgSO4. The solvent was evaporated in vacuo and the crude product was purified by column chromatography with a mixture of n-hexane:ethyl acetate (1:1) as the eluent.

후처리

  1. customwas consumed (monitored by TLC)
  2. additionThen the mixture was poured onto ice water (50 ml)
  3. extractionthe aqueous phase was extracted with ethyl acetate (3×30 ml)
  4. washThe combined organic phases were washed with water
  5. dry with materialdried over anhydrous MgSO4
  6. customThe solvent was evaporated in vacuo
  7. customthe crude product was purified by column chromatography with a mixture of n-hexane:ethyl acetate (1:1) as the eluent

출처 및 근거

ORD 기록
ord-36c7cc926e514e7ea932e77118df6091
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536210B2

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