Hydrochloric Acid → N-{[2-chloro-3-(trifluoromethyl)phenyl]methyl}-3-methyl-2-oxo-1-(4-piperidinyl)-4-imidazolidinecarboxamide hydrochloride

HRID 2080964노트

반응식

HRID 2080964 반응식
[Cl:1][C:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:12][NH:13][C:14]([CH:16]1[CH2:20][N:19]([CH:21]2[CH2:26][CH2:25][N:24](C(OC(C)(C)C)=O)[CH2:23][CH2:22]2)[C:18](=[O:34])[N:17]1[CH3:35])=[O:15].Cl>O1CCOCC1>[ClH:1].[Cl:1][C:2]1[C:7]([C:8]([F:9])([F:11])[F:10])=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:12][NH:13][C:14]([CH:16]1[CH2:20][N:19]([CH:21]2[CH2:22][CH2:23][NH:24][CH2:25][CH2:26]2)[C:18](=[O:34])[N:17]1[CH3:35])=[O:15]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 671035531,1-Dimethylethyl 4-{4-[({[2-chloro-3-(trifluoromethyl)phenyl]methyl}amino)carbonyl]-3-methyl-2-oxo-1-imidazolidinyl}-1-piperidinecarboxylate

생성물 1

HCID 67103577N-{[2-chloro-3-(trifluoromethyl)phenyl]methyl}-3-methyl-2-oxo-1-(4-piperidinyl)-4-imidazolidinecarboxamide hydrochloride수율 160%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

A solution of 1,1-dimethylethyl 4-{4-[({[2-chloro-3-(trifluoromethyl)phenyl]methyl}amino)carbonyl]-3-methyl-2-oxo-1-imidazolidinyl}-1-piperidinecarboxylate (218 mg, 0.42 mmol) in 1,4-dioxane (3 ml) was treated with 4M hydrogen chloride in 1,4-dioxane (1 ml) and the reaction was stirred at room temperature for 4 hours. The solvent was evaporated and the gum was dissolved in methanol and the solvent evaporated. The residue was triturated with ether and the solid was collected and dried to give N-{[2-chloro-3-(trifluoromethyl)phenyl]methyl}-3-methyl-2-oxo-1-(4-piperidinyl)-4-imidazolidinecarboxamide hydrochloride (153 mg, 80%), LC/MS [M+H]+=419, retention time=1.75 minutes.

후처리

  1. customThe solvent was evaporated
  2. dissolutionthe gum was dissolved in methanol
  3. customthe solvent evaporated
  4. customThe residue was triturated with ether
  5. customthe solid was collected
  6. customdried

출처 및 근거

ORD 기록
ord-ea2cf188e1fb485293288c8594545ada
출처 데이터셋
uspto-grants-2011_04
특허 번호
US07932282B2

반응 노트

불러오는 중…