Hydrogen Sulfide → Ethyl 2-carbamothioylnicotinate

HRID 1400222노트

반응식

HRID 1400222 반응식
CCN(CC)CC.[C:8]([C:10]1[N:20]=[CH:19][CH:18]=[CH:17][C:11]=1[C:12]([O:14][CH2:15][CH3:16])=[O:13])#[N:9].[SH2:21]>N1C=CC=CC=1>[C:8]([C:10]1[N:20]=[CH:19][CH:18]=[CH:17][C:11]=1[C:12]([O:14][CH2:15][CH3:16])=[O:13])(=[S:21])[NH2:9]

참가 물질

5

반응물 3

HCID 402Hydrogen SulfideHCID 8471TriethylamineHCID 12747366Ethyl 2-cyanopyridine-3-carboxylate

생성물 1

HCID 86644784Ethyl 2-carbamothioylnicotinate

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

Et3N (10 ml) was added to a solution of ethyl 2-cyanonicotinate (1.9 g, 10.78 mmol) in 20 ml of pyridine. Hydrogen sulfide was passed through the reaction mixture at 5° C. for 20 minutes, then the mixture was stirred for 1 hour at room temperature. For work up the solution was purged with nitrogen for 30 minutes, evaporated to dryness, and the remaining solid dissolved in 200 ml of dichloromethane. The organic layer was washed successively with water and brine, dried, evaporated and treated with ethylacetate to give 2.15 g of a red oil which was reacted without further purification.

후처리

  1. customFor work up the solution was purged with nitrogen for 30 minutes
  2. customevaporated to dryness
  3. dissolutionthe remaining solid dissolved in 200 ml of dichloromethane
  4. washThe organic layer was washed successively with water and brine
  5. customdried
  6. customevaporated
  7. additiontreated with ethylacetate

출처 및 근거

ORD 기록
ord-5123d939dd004b7abf47a487f5fac4b0
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08906941B2

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