Water → 1-[1-(1-methoxycarbonylpiperidin-4-yl)-piperidin-4-yl]-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one

HRID 47534노트

반응식

HRID 47534 반응식
N[C:2]1[C:3]([NH:8][CH:9]2[CH2:14][CH2:13][N:12]([CH:15]3[CH2:20][CH2:19][N:18](C(OC)=O)[CH2:17][CH2:16]3)[CH2:11][CH2:10]2)=[N:4][CH:5]=[CH:6][CH:7]=1.ClC(Cl)(O[C:29](=[O:35])[O:30][C:31](Cl)(Cl)Cl)Cl.C([N:39]([CH2:42]C)CC)C.[OH2:44]>O1CCCC1>[CH3:31][O:30][C:29]([N:18]1[CH2:17][CH2:16][CH:15]([N:12]2[CH2:11][CH2:10][CH:9]([N:8]3[C:6]4[C:5](=[N:39][CH:42]=[CH:2][CH:7]=4)[NH:4][C:3]3=[O:44])[CH2:14][CH2:13]2)[CH2:20][CH2:19]1)=[O:35]

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 94429TriphosgeneHCID 227452603-Amino-2-[1-(1-methoxycarbonylpiperidin-4-yl)-piperidin-4-yl]aminopyridin

생성물 1

HCID 227452991-[1-(1-methoxycarbonylpiperidin-4-yl)-piperidin-4-yl]-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Twenty (20) mg of 3-amino-2-[1-(1-methoxycarbonylpiperidin-4-yl)piperidin-4-yl]aminopyridin and 18 mg of triphosgene were dissolved in 2 ml of tetrahydrofuran, and to which 45 μl of triethylamine was added under cooling with ice. The system was further stirred at the same temperature for 2 hours and for an hour, at room temperature. Thereafter water was added to the reaction liquid and extracted with chloroform. The extract was dried over anhydrous sodium sulfate, concentrated and the resulting crude product was purified by silica gel chromatography (chloroform/methanol=10/1) to give 12 mg of the title compound.

후처리

  1. temperatureunder cooling with ice
  2. extractionextracted with chloroform
  3. dry with materialThe extract was dried over anhydrous sodium sulfate
  4. concentrationconcentrated
  5. customthe resulting crude product was purified by silica gel chromatography (chloroform/methanol=10/1)

출처 및 근거

ORD 기록
ord-51729313193b4899bcf2d02b4d802fee
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06699880B1

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