Hydrochloric Acid → Acetamide, N-(4-aminocyclohexyl)-, hydrochloride (1:1)

HRID 2386674노트

반응식

HRID 2386674 반응식
[ClH:1].C(OC(=O)[NH:8][CH:9]1[CH2:14][CH2:13][CH:12]([NH:15][C:16](=[O:18])[CH3:17])[CH2:11][CH2:10]1)(C)(C)C>CO>[ClH:1].[NH2:8][CH:9]1[CH2:10][CH2:11][CH:12]([NH:15][C:16](=[O:18])[CH3:17])[CH2:13][CH2:14]1

참가 물질

4

반응물 2

HCID 313Hydrochloric Acid2회HCID 66955585tert-Butyl (1R*,4R*)-4-acetamidocyclohexylcarbamate

생성물 1

HCID 66728468Acetamide, N-(4-aminocyclohexyl)-, hydrochloride (1:1)

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

HCl (2.0 M in MeOH, 200 mL) was added to a suspension of (4-acetylamino-cyclohexyl)-carbamic acid tert-butyl ester (14.3 g) in MeOH (100 mL) and the resulting mixture was stirred at RT for 18 h. A second aliquot of HCl (2.0 M in MeOH, 100 mL) was then added and the resulting mixture was stirred at RT overnight. The reaction mixture was then concentrated under reduced pressure and the residue was triturated with Et2O. The very hygroscopic solid was collected by filtration after treatment with toluene, was then dried at 50° C. under reduced pressure to afford 12.46 g of N-(4-amino-cyclohexyl)-acetamide hydrochloride.

후처리

  1. stirringthe resulting mixture was stirred at RT overnight
  2. concentrationThe reaction mixture was then concentrated under reduced pressure
  3. customthe residue was triturated with Et2O
  4. filtrationThe very hygroscopic solid was collected by filtration after treatment with toluene
  5. customwas then dried at 50° C. under reduced pressure

출처 및 근거

ORD 기록
ord-4bcafc2f75bd4f08b554ff419407b961
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08268840B2

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