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4-Methylmorpholine → rac-Methyl 4,4,4-trifluoro-2-[({8-[(3-fluoropyridin-2-yl)methoxy]-2,6-dimethylimidazo[1,2-a]pyridin-3-yl}carbonyl)amino]butanoate

HRID 1844188
ノート
印刷プレビュー

反応式

HRID 1844188 の反応式
Cl.[F:2][C:3]1[C:4]([CH2:9][O:10][C:11]2[C:12]3[N:13]([C:18]([C:22](O)=[O:23])=[C:19]([CH3:21])[N:20]=3)[CH:14]=[C:15]([CH3:17])[CH:16]=2)=[N:5][CH:6]=[CH:7][CH:8]=1.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.CN1CCOCC1.Cl.[NH2:55][CH:56]([CH2:61][C:62]([F:65])([F:64])[F:63])[C:57]([O:59][CH3:60])=[O:58]>CN(C=O)C.O>[F:63][C:62]([F:64])([F:65])[CH2:61][CH:56]([NH:55][C:22]([C:18]1[N:13]2[CH:14]=[C:15]([CH3:17])[CH:16]=[C:11]([O:10][CH2:9][C:4]3[C:3]([F:2])=[CH:8][CH:7]=[CH:6][N:5]=3)[C:12]2=[N:20][C:19]=1[CH3:21])=[O:23])[C:57]([O:59][CH3:60])=[O:58]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 79724-MethylmorpholineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 44717559Methyl 2-amino-4,4,4-trifluorobutanoate hydrochlorideHCID 867182148-[(3-Fluoropyridin-2-yl)methoxy]-2,6-dimethylimidazo[1,2-a]pyridine-3-carboxylic acid hydrochloride

生成物 1

HCID 90115188
rac-Methyl 4,4,4-trifluoro-2-[({8-[(3-fluoropyridin-2-yl)methoxy]-2,6-dimethylimidazo[1,2-a]pyridin-3-yl}carbonyl)amino]butanoate

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

250 mg (0.71 mmol) of 8-[(3-fluoropyridin-2-yl)methoxy]-2,6-dimethylimidazo[1,2-a]pyridine-3-carboxylic acid hydrochloride from Example 121A were initially charged in 4.1 ml of DMF, and 274 mg (0.85 mmol) of TBTU and 0.47 ml (4.26 mmol) of 4-methylmorpholine were added. 221 mg (1.07 mmol) of methyl 2-amino-4,4,4-trifluorobutanoate hydrochloride from Example 75A were then added, and the reaction mixture was stirred at RT overnight. About 32 ml of water were added to the mixture. The precipitated solid was filtered off, washed with water and dried under high vacuum. This gave 298 mg (68% of theory, purity 76%) of the target compound.

後処理

  1. filtrationThe precipitated solid was filtered off
  2. washwashed with water
  3. customdried under high vacuum

出典と根拠

ORDレコード
ord-efe2350f430846acb1770d6bca50559f
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08946215B2

反応ノート

読み込み中…

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