Thioacetamide → 2-Methyl-5,6-dihydrobenzo[d]thiazol-7(4H)-one

HRID 2371047ノート

反応式

HRID 2371047 の反応式
[C:1](=[S:4])([NH2:3])[CH3:2].Br[CH:6]1[C:11](=[O:12])[CH2:10][CH2:9][CH2:8][C:7]1=O>C(O)C>[CH3:2][C:1]1[S:4][C:10]2[C:11](=[O:12])[CH2:6][CH2:7][CH2:8][C:9]=2[N:3]=1

参加物

4

反応物 2

HCID 2723949ThioacetamideHCID 27704762-Bromocyclohexane-1,3-dione

生成物 1

HCID 149133692-Methyl-5,6-dihydrobenzo[d]thiazol-7(4H)-one

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of ethanethioamide (0.75 g, 10 mmol) in ethanol (20 mL) at room temperature was added 2-bromocyclohexane-1,3-dione (1.9 g, 10 mmol) in portions. The reaction solution was refluxed for 2 hours while stirring. After removal of solvents, the residue was diluted with water and washed with diethyl ether. The separated aqueous layer was basified with sodium carbonate solution. The resulting solid was collected by vacuum filtration, rinsed with water. The solid was suspended in methanol and followed by evaporation to dryness to produce the title compound.

後処理

  1. temperatureThe reaction solution was refluxed for 2 hours
  2. customAfter removal of solvents
  3. additionthe residue was diluted with water
  4. washwashed with diethyl ether
  5. filtrationThe resulting solid was collected by vacuum filtration
  6. washrinsed with water
  7. customfollowed by evaporation to dryness

出典と根拠

ORDレコード
ord-ce6dc72c650a4d18bcf495da9bdd852e
出典データセット
uspto-grants-2014_04
特許番号
US08710245B2

反応ノート

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