Hydrochloric Acid → 4-Aminocyclohexane-1-sulfonamide

HRID 1483837ノート

反応式

HRID 1483837 の反応式
O=C1C2C(=CC=CC=2)C(=O)[N:3]1[CH:12]1[CH2:17][CH2:16][CH:15]([S:18]([NH2:21])(=[O:20])=[O:19])[CH2:14][CH2:13]1.Cl>CCO>[NH2:3][CH:12]1[CH2:17][CH2:16][CH:15]([S:18]([NH2:21])(=[O:19])=[O:20])[CH2:14][CH2:13]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 712276614-(1,3-Dioxoisoindolin-2-yl)cyclohexane-1-sulfonamide

生成物 1

HCID 893898974-Aminocyclohexane-1-sulfonamide収率 40.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 4-(1,3-dioxoisoindolin-2-yl)cyclohexane-1-sulfonamide (3 g, 9.7 mmol) and NH2NH2H2O (1 mL) in EtOH (15 mL) was heated at reflux for 30 min. After cooling, the pH was adjusted with diluted HCl to 5. The mixture was concentrated in vacuo. The residue was dissipated with 35% HCl (10 mL) and heating until all solid material was dissolved. Upon cooling, a crystalline material was filtered and the filtrated was concentrated to give crude 4-aminocyclohexane-1-sulfonamide (700 mg, 40%) as a yellow solid, which was used in the next step directly.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 30 min
  3. temperatureAfter cooling
  4. concentrationThe mixture was concentrated in vacuo
  5. temperatureheating until all solid material
  6. dissolutionwas dissolved
  7. temperatureUpon cooling
  8. filtrationa crystalline material was filtered
  9. concentrationthe filtrated was concentrated

出典と根拠

ORDレコード
ord-ef1803ba20484ee4ae800665696834c8
出典データセット
uspto-grants-2016_08
特許番号
US09416132B2

反応ノート

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