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1-Pyrrolidinamine → HCID 86636478, 화합물

HRID 1666600
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HRID 1666600 반응식
NN1CCCC1.[CH3:7][N:8]([CH3:29])[C:9]([CH:11]1[CH2:16][CH2:15][N:14]([C:17]2[C:26]3[C:21](=[CH:22][C:23]([F:27])=[CH:24][CH:25]=3)[N:20]=[C:19]([Cl:28])[N:18]=2)[CH2:13][CH2:12]1)=[O:10].Cl.[NH2:31][C@H:32]1[CH2:36][CH2:35][N:34]([C:37](=[O:50])[CH2:38][C:39]2[CH:44]=[CH:43][C:42]([O:45][C:46]([F:49])([F:48])[F:47])=[CH:41][CH:40]=2)[CH2:33]1.C(N(CC)C(C)C)(C)C>C(Cl)(Cl)Cl.C(=O)([O-])O.[Na+].C(O)CCC>[ClH:28].[CH3:7][N:8]([CH3:29])[C:9]([CH:11]1[CH2:16][CH2:15][N:14]([C:17]2[C:26]3[C:21](=[CH:22][C:23]([F:27])=[CH:24][CH:25]=3)[N:20]=[C:19]([NH:31][C@H:32]3[CH2:36][CH2:35][N:34]([C:37](=[O:50])[CH2:38][C:39]4[CH:40]=[CH:41][C:42]([O:45][C:46]([F:47])([F:48])[F:49])=[CH:43][CH:44]=4)[CH2:33]3)[N:18]=2)[CH2:13][CH2:12]1)=[O:10]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 279461-PyrrolidinamineHCID 81531DiisopropylethylamineHCID 57970126HCID 57970126, 화합물HCID 86636479(S)-1-(3-aminopyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone mono hydrochloride

생성물 1

HCID 86636478HCID 86636478, 화합물수율 23.7%

시약·촉매·용매 3

HCID 263
1-Butanol
용매
HCID 6212Chloroform용매
HCID 516892Sodium Bicarbonate용매

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온도
120 °C

실험 절차

A mixture of 2,4-dichloro-7-fluoroquinazoline (250 mg), piperidine-4-carboxylic acid dimethylamide (189 mg), triethylamine (0.24 mL), THF (6 mL), and DMF (4 mL) was stirred at room temperature for 13 h. The reaction mixture was diluted with a mixture of chloroform and saturated aqueous sodium hydrogencarbonate, and then the aqueous layer was extracted 3 times with chloroform. The organic layer was dried with anhydrous sodium sulfate, the desiccant was removed by filtration, the filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane/ethyl acetate=7:3) to obtain colorless solid 1-(2-chloro-7-fluoroquinazolin-4-yl)piperidine-4-carboxylic acid dimethylamide (407 mg). (2) A mixture of 1-(2-chloro-7-fluoroquinazolin-4-yl)piperidine-4-carboxylic acid dimethylamide (250 mg), 1-((S)-3-aminopyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone mono hydrochloride (265 mg), N,N-diisopropylethylamine (0.32 mL), and n-butanol (1.2 mL) was heated at 120° C. for 57 h with stirring. The reaction mixture was diluted with a mixture of chloroform and saturated aqueous sodium hydrogencarbonate, and then the aqueous layer was extracted with chloroform. The organic layer was dried with anhydrous sodium sulfate, the desiccant was removed by filtration, the filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (NH silica gel, hexane/ethyl acetate=4:1−ethyl acetate, and silica gel, chloroform/methanol=95:5). The resulting purification product was dissolved in ethyl acetate (2.0 mL), followed by addition of a solution (0.1 mL) of 4 M HCl in ethyl acetate, and the mixture was stirred at room temperature for 3.5 h. The solvent was evaporated under reduced pressure to obtain the amorphous title compound (110 mg).

후처리

  1. extractionthe aqueous layer was extracted with chloroform
  2. dry with materialThe organic layer was dried with anhydrous sodium sulfate
  3. customthe desiccant was removed by filtration
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customthe residue was purified by silica gel column chromatography (NH silica gel, hexane/ethyl acetate=4:1−ethyl acetate, and silica gel, chloroform/methanol=95:5)
  6. customThe resulting purification product
  7. dissolutionwas dissolved in ethyl acetate (2.0 mL)
  8. additionfollowed by addition of a solution (0.1 mL) of 4 M HCl in ethyl acetate
  9. stirringthe mixture was stirred at room temperature for 3.5 h
  10. customThe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-c11da105693044f4b75eabd9408079ea
출처 데이터셋
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08044068B2

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