Hydrochloric Acid → HCID 59336110, 화합물

HRID 2359506노트

반응식

HRID 2359506 반응식
Cl.[CH:2]1([CH2:8][N:9]2[CH2:14][CH2:13][CH:12]([N:15]([CH3:36])[C:16](=[O:35])[CH2:17][O:18][C:19]3[N:24]=[C:23]([CH3:25])[C:22]([NH:26]C(=O)OC(C)(C)C)=[C:21]([CH3:34])[N:20]=3)[CH2:11][CH2:10]2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.[OH-].[Na+]>C(Cl)(Cl)Cl>[NH2:26][C:22]1[C:23]([CH3:25])=[N:24][C:19]([O:18][CH2:17][C:16]([N:15]([CH:12]2[CH2:13][CH2:14][N:9]([CH2:8][CH:2]3[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]3)[CH2:10][CH2:11]2)[CH3:36])=[O:35])=[N:20][C:21]=1[CH3:34]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 59336176Tert-butyl 2-(2-((1-(cyclohexylmethyl)piperidine-4-yl)(methyl)amino)-2-oxoethoxy)-4,6-dimethylpyrimidine-5-ylcarbamate

생성물 1

HCID 59336110HCID 59336110, 화합물수율 76%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

6N HCl (0.7 mL) was added to a chloroform (0.5 mL) solution of Compound 32 (39 mg) and the mixture was stirred at room temperature for 1 hour. While the reaction mixture was cooled with ice, a 4N aqueous sodium hydroxide solution was added to neutralize the mixture. The resulting product was extracted with chloroform and the organic layer was dried over sodium sulfate, filtered, and concentrated under reduced pressure. The resulting residue was purified by amino-coated silica gel (Fuji Sylysia Chemical Ltd., NH-DM1020) column chromatography (ethyl acetate) to give 23 mg (76% yield) of the title compound.

후처리

  1. temperatureWhile the reaction mixture was cooled with ice
  2. extractionThe resulting product was extracted with chloroform
  3. dry with materialthe organic layer was dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting residue was purified by amino-coated silica gel (Fuji Sylysia Chemical Ltd., NH-DM1020) column chromatography (ethyl acetate)

출처 및 근거

ORD 기록
ord-0f1084de570246bcb813f4eaea689527
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08685989B2

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