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

HRID 493124ノート

反応式

HRID 493124 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6212Chloroform溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-0004a56d53d64d0baae3855f59176ad0
出典データセット
uspto-grants-2009_05
特許番号
US07534793B2

反応ノート

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