Isobutyryl chloride → N-Carbamothioyl-2-methylpropanamide

HRID 869394ノート

反応式

HRID 869394 の反応式
[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]

参加物

4

反応物 2

HCID 62325Isobutyryl chlorideHCID 2723790Thiourea

生成物 1

HCID 3555130N-Carbamothioyl-2-methylpropanamide収率 30.8%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-7ee250a5b8ca490791fd07500fa941c9
出典データセット
uspto-grants-2015_03
特許番号
US08969373B2

反応ノート

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