Hydrochloric Acid → N,N'-Dimethyl-N-(5-methyl-3-pyridyl)ethane-1,2-diamine dihydrochloride

HRID 631824노트

반응식

HRID 631824 반응식
[CH3:1][N:2]([CH2:10][CH2:11][N:12]([CH3:20])[C:13]1[CH:14]=[N:15][CH:16]=[C:17]([CH3:19])[CH:18]=1)C(=O)OC(C)(C)C.[ClH:21]>C(Cl)Cl>[ClH:21].[ClH:21].[CH3:20][N:12]([C:13]1[CH:14]=[N:15][CH:16]=[C:17]([CH3:19])[CH:18]=1)[CH2:11][CH2:10][NH:2][CH3:1]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 131735429tert-Butyl N-methyl-N-[2-[methyl-(5-methyl-3-pyridyl)amino]ethyl]carbamate

생성물 1

HCID 89825869N,N'-Dimethyl-N-(5-methyl-3-pyridyl)ethane-1,2-diamine dihydrochloride

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

tert-Butyl N-methyl-N-[2-[methyl-(5-methyl-3-pyridyl)amino]ethyl]carbamate (301 mg, 1.078 mmol) was dissolved in DCM (40 ml). Hydrochloric acid (4M in dioxane, 5.4 ml) was added and the mixture was stirred at room temperature for 48 hours. The mixture was concentrated under reduced pressure, diethylether was added and the mixture was stirred at room temperature for 4 days. The solids were collected by filtration, rinsed with diethylether and dried under reduced pressure to yield 199 mg (0.789 mmol, 73%) MS(ESI) m/z=180.2 [M+1]+.

후처리

  1. concentrationThe mixture was concentrated under reduced pressure, diethylether
  2. additionwas added
  3. stirringthe mixture was stirred at room temperature for 4 days
  4. filtrationThe solids were collected by filtration
  5. washrinsed with diethylether
  6. customdried under reduced pressure
  7. customto yield 199 mg (0.789 mmol, 73%) MS(ESI) m/z=180.2 [M+1]+

출처 및 근거

ORD 기록
ord-82ca38c6695d4dd8a0c6239fa6d85901
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09321724B2

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