Potassium Carbonate → 1,2,3,4-Tetrahydro-3-methyl-1-(2-methylpropyl)-2,4-dioxo-5-(thien-2-ylthio)-thieno[2,3-d]pyrimidine-6-carboxaldehyde

HRID 379595노트

반응식

HRID 379595 반응식
Cl[C:2]1[C:10]2[C:9](=[O:11])[N:8]([CH3:12])[C:7](=[O:13])[N:6]([CH2:14][CH:15]([CH3:17])[CH3:16])[C:5]=2[S:4][C:3]=1[CH:18]=[O:19].C(=O)([O-])[O-].[K+].[K+].[S:26]1[CH:30]=[CH:29][CH:28]=[C:27]1[SH:31]>CC(C)=O>[CH3:12][N:8]1[C:9](=[O:11])[C:10]2[C:2]([S:31][C:27]3[S:26][CH:30]=[CH:29][CH:28]=3)=[C:3]([CH:18]=[O:19])[S:4][C:5]=2[N:6]([CH2:14][CH:15]([CH3:17])[CH3:16])[C:7]1=[O:13]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 5226742-ThiophenethiolHCID 183666245-Chloro-1,2,3,4-tetrahydro-3-methyl-1-(2-methylpropyl)-2,4-dioxo-thieno[2,3-d]pyrimidine-6-carboxaldehyde

생성물 1

HCID 183665901,2,3,4-Tetrahydro-3-methyl-1-(2-methylpropyl)-2,4-dioxo-5-(thien-2-ylthio)-thieno[2,3-d]pyrimidine-6-carboxaldehyde

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To a solution of 5-chloro-1,2,3,4-tetrahydro-3-methyl-1-(2-methylpropyl)-2,4-dioxo-thieno[2,3-d]pyrimidine-6-carboxaldehyde in acetone (30 ml) was added potassium carbonate (0.402 g) followed by 2-thiophene thiol (0.337 g). The reaction was stirred for 24 hours under nitrogen. The acetone was evaporated and the resulting residue was partitioned between ethyl acetate and water (1:1, 50 ml in total). The aqueous phase was extracted twice with ethyl acetate (25 ml) The organic extracts were washed with brine, then dried over magnesium sulfate, filtered and evaporated to leave a brown oil. This oil was triturated with diethyl ether to give the subtitle compound as a pale brown solid (0.528 g).

후처리

  1. customThe acetone was evaporated
  2. customthe resulting residue was partitioned between ethyl acetate and water (1:1, 50 ml in total)
  3. extractionThe aqueous phase was extracted twice with ethyl acetate (25 ml) The organic extracts
  4. washwere washed with brine
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. customevaporated
  8. customto leave a brown oil
  9. customThis oil was triturated with diethyl ether

출처 및 근거

ORD 기록
ord-1abd861ae7a4454e920711dcf3e83dc4
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06300334B1

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