Potassium Carbonate → 4-tert-Butyloxycarbonylamino-1-(6-methoxy-[1,5]naphthyridin-4-yl)aminocarbonylpiperidine

HRID 493124노트

반응식

HRID 493124 반응식
[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([O:12][CH3:13])[N:10]=2)[N:5]=[CH:4][CH:3]=1.C1N=CN([C:19]([N:21]2[CH:25]=N[CH:23]=[CH:22]2)=[O:20])C=1.Cl.[C:27]([O:31][C:32]([NH:34][CH:35]1CCNC[CH2:36]1)=[O:33])([CH3:30])([CH3:29])[CH3:28].C(=O)([O-])[O-].[K+].[K+]>CN(C)C1C=CN=CC=1.C(Cl)(Cl)Cl>[C:27]([O:31][C:32]([NH:34][CH:35]1[CH2:23][CH2:22][N:21]([C:19]([NH:1][C:2]2[C:11]3[C:6](=[CH:7][CH:8]=[C:9]([O:12][CH3:13])[N:10]=3)[N:5]=[CH:4][CH:3]=2)=[O:20])[CH2:25][CH2:36]1)=[O:33])([CH3:30])([CH3:29])[CH3:28]

참가 물질

7

반응물 4

HCID 11430Potassium CarbonateHCID 682631,1'-CarbonyldiimidazoleHCID 27560284-(tert-Butoxycarbonylamino)piperidine hydrochlorideHCID 114352366-Methoxy-1,5-naphthyridin-4-amine

생성물 1

HCID 222817154-tert-Butyloxycarbonylamino-1-(6-methoxy-[1,5]naphthyridin-4-yl)aminocarbonylpiperidine

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6212Chloroform용매

실험 절차

To a solution of 4-amino-6-methoxy-[1,5]naphthyridine (Example 400a) (2.1 g, 13.5 mmol) and 4-(dimethylamino)pyridine (1.62 g) in anhydrous chloroform (45 ml) was added N,N-carbonyldiimidazole (3.28 g, 20.1 mmol). The mixture was stirred for 4 h at room temperature, then evaporated and the residue was dissolved in anhydrous DMF (45 ml). 4-tert-Butoxycarbonylaminopiperidine hydrochloride (3.34 g, 13.5 mmol) and potassium carbonate (1.89 g) were added, and the mixture was heated at 70° C. overnight. The mixture was evaporated and the residue was mixed with water (120 ml). The solid was filtered off and dried (3.89 g).

후처리

  1. customevaporated
  2. dissolutionthe residue was dissolved in anhydrous DMF (45 ml)
  3. temperaturethe mixture was heated at 70° C. overnight
  4. customThe mixture was evaporated
  5. additionthe residue was mixed with water (120 ml)
  6. filtrationThe solid was filtered off
  7. customdried (3.89 g)

출처 및 근거

ORD 기록
ord-0004a56d53d64d0baae3855f59176ad0
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07534793B2

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