Hydrochloric Acid → 4-Aminocyclohexane-1-sulfonamide

HRID 1483837노트

반응식

HRID 1483837 반응식
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

참가 물질

4

반응물 2

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

생성물 1

HCID 893898974-Aminocyclohexane-1-sulfonamide수율 40.5%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ef1803ba20484ee4ae800665696834c8
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09416132B2

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