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Acetic Acid → 5-Cyclohexyl 3-methylamino 4,5,6,7-tetrahydro indazole

HRID 1284013
ノート
印刷プレビュー

反応式

HRID 1284013 の反応式
[CH:1]1([CH:7]2[CH2:12][CH2:11][C:10](=O)[CH:9]([C:14](=S)[NH:15][CH3:16])[CH2:8]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.O.[NH2:19][NH2:20].C(O)(=O)C.CCOCC>C(O)C>[CH:1]1([CH:7]2[CH2:12][CH2:11][C:10]3[NH:20][N:19]=[C:14]([NH:15][CH3:16])[C:9]=3[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

6

反応物 4

HCID 176Acetic AcidHCID 3283Diethyl EtherHCID 24654Hydrazine hydrate (1:1)HCID 215152814-Cyclohexyl 2-methylthiocarbamoyl cyclohexanone

生成物 1

HCID 215152845-Cyclohexyl 3-methylamino 4,5,6,7-tetrahydro indazole

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

0.7 g of 4-cyclohexyl 2-methylthiocarbamoyl cyclohexanone dissolved in 30 ml ethanol are added with 0.15 g hydrazine hydrate. The mixture is heated to reflux for 30 mn until the evolution of sulphydric gas has ceased. 0.3 ml acetic acid are thereafter added and the whole is refluxed for 3 hours. The mixture is evaporated off giving a yellow liquid as residue. The residue is taken up with ether; the organic solution is washed with a saturated aqueous solution of sodium bicarbonate then with water until the washings are neutral, finally dried and evaporated off. 0.6 g of 5-cyclohexyl 3-methylamino 4,5,6,7-tetrahydroindazole are thus recovered and recrystallized from the minimum amount of isopropanol.

後処理

  1. temperatureThe mixture is heated
  2. temperatureto reflux for 30 mn until the evolution of sulphydric gas
  3. temperaturethe whole is refluxed for 3 hours
  4. customThe mixture is evaporated off
  5. customgiving a yellow liquid as residue
  6. washthe organic solution is washed with a saturated aqueous solution of sodium bicarbonate
  7. customfinally dried
  8. customevaporated off
  9. custom0.6 g of 5-cyclohexyl 3-methylamino 4,5,6,7-tetrahydroindazole are thus recovered
  10. customrecrystallized from the minimum amount of isopropanol

出典と根拠

ORDレコード
ord-5c95b3b7eac4496dab84dc969a03bfe7
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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