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Hydrochloric Acid → 4-Cyclohexyl 2-methylthiocarbamoyl cyclohexanone

HRID 1284012
ノート
印刷プレビュー

反応式

HRID 1284012 の反応式
[CH:1]1([CH:7]2[CH2:12][CH2:11][C:10](N3CCOCC3)=[C:9]([C:19](=[S:22])[NH:20][CH3:21])[CH2:8]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.Cl.[OH2:24]>C(O)C>[CH:1]1([CH:7]2[CH2:12][CH2:11][C:10](=[O:24])[CH:9]([C:19](=[S:22])[NH:20][CH3:21])[CH2:8]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 215153064-Cyclohexyl 2-methylthiocarbamoyl 1-morpholyl cyclohex-1 ene

生成物 1

HCID 215152814-Cyclohexyl 2-methylthiocarbamoyl cyclohexanone

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

1 g of 4-cyclohexyl 2-methylthiocarbamoyl 1-morpholyl cyclohex-1 ene is dissolved in 20 ml ethanol at room temperature. To this solution 2 ml 4 N hydrochloric acid solution are added and the mixture becomes pale yellow. The reaction mixture is kept under stirring for 1/2 hour. 60 ml water are then added and a brownish-red precipitate appears. It is sucction-filtered, washed with water and further taken up in benzene until complete solution. The benzenic solution is dried, filtered and evaporated to dryness. The dry residue is further washed with water then taken up with benzene. After distillation of the solvent 0.7 g of 4-cyclohexyl 2-methyl thio carbamoyl cyclohexanone are thus obtained which is used as such for the next step of the synthesis.

後処理

  1. filtrationIt is sucction-filtered
  2. washwashed with water
  3. customThe benzenic solution is dried
  4. filtrationfiltered
  5. customevaporated to dryness
  6. washThe dry residue is further washed with water
  7. distillationAfter distillation of the solvent 0.7 g of 4-cyclohexyl 2-methyl thio carbamoyl cyclohexanone
  8. customare thus obtained which
  9. customsuch for the next step of the synthesis

出典と根拠

ORDレコード
ord-5cc9847bc7a3492e99104a446d59fbea
出典データセット
uspto-grants-1976_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03978044

反応ノート

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