Isobutyryl chloride → N-Carbamothioyl-2-methylpropanamide

HRID 869394노트

반응식

HRID 869394 반응식
[NH2:1][C:2]([NH2:4])=[S:3].[C:5](Cl)(=[O:9])[CH:6]([CH3:8])[CH3:7]>C1(C)C=CC=CC=1>[C:5]([NH:1][C:2]([NH2:4])=[S:3])(=[O:9])[CH:6]([CH3:8])[CH3:7]

참가 물질

4

반응물 2

HCID 62325Isobutyryl chlorideHCID 2723790Thiourea

생성물 1

HCID 3555130N-Carbamothioyl-2-methylpropanamide수율 30.8%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Thiourea (152 g, 2 mol) was dissolved in toluene (1520 mL). To the solution was added isobutyryl chloride (213 g, 2 mol) under mechanical stirring. The reaction mixture was refluxed for 3 hours. TLC monitored the reaction. After the reaction completed, the reaction mixture was cooled to room temperature and filtered to remove insoluble solids. The filtrate was concentrated to dryness. The yellow solids were collected by filtration, washed with petroleum ether (100 mL×3) to appear white, dried in vacumm to give the desired product 11A (90 g, 30% yield) as a white solid (mp: 114˜116° C.).

후처리

  1. temperatureThe reaction mixture was refluxed for 3 hours
  2. customthe reaction
  3. filtrationfiltered
  4. customto remove insoluble solids
  5. concentrationThe filtrate was concentrated to dryness
  6. filtrationThe yellow solids were collected by filtration
  7. washwashed with petroleum ether (100 mL×3)
  8. customdried in vacumm

출처 및 근거

ORD 기록
ord-7ee250a5b8ca490791fd07500fa941c9
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08969373B2

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