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Sodium Carbonate → HCID 58447855、化合物

HRID 1036213
ノート
印刷プレビュー

反応式

HRID 1036213 の反応式
[N:1]1[CH:6]=[CH:5][C:4]([C:7]2[CH:8]=[CH:9][C:10]([NH2:13])=[N:11][CH:12]=2)=[CH:3][N:2]=1.[CH3:14][C:15]1[CH:16]=[C:17]([CH2:27][C:28](O)=[O:29])[CH:18]=[CH:19][C:20]=1[C:21]1[CH:26]=[CH:25][N:24]=[N:23][CH:22]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C.C([O-])([O-])=O.[Na+].[Na+]>CN(C=O)C.C(OCC)(=O)C>[CH3:14][C:15]1[CH:16]=[C:17]([CH2:27][C:28]([NH:13][C:10]2[CH:9]=[CH:8][C:7]([C:4]3[CH:5]=[CH:6][N:1]=[N:2][CH:3]=3)=[CH:12][N:11]=2)=[O:29])[CH:18]=[CH:19][C:20]=1[C:21]1[CH:26]=[CH:25][N:24]=[N:23][CH:22]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 10340Sodium CarbonateHCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 57821650HCID 57821650、化合物HCID 58447649HCID 58447649、化合物

生成物 1

HCID 58447855
HCID 58447855、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 5-(pyridazin-4-yl)pyridin-2-amine 134-1 (53 mg, 0.31 mmol), 2-(3-methyl-4-(pyridazin-4-yl)phenyl)acetic acid 134-3 (73 mg, 0.32 mmol), HATU (122 mg, 0.32 mmol) and DIEA (80 uL, 0.46 mmol) in DMF (1.0 ml) was stirred at room temperature overnight. Then it was distributed between ethyl acetate (40 ml) and 3% Na2CO3 aqueous solution (40 ml) and extracted with 0.5 N HCl solution (30 ml). The aqueous extraction was treated with Na2CO3 to adjust the pH to around 10 followed by extraction with ethyl acetate (30 ml×2). The combined organic extractions were dried over Na2SO4 and concentrated by evaporation. The residue was subjected to reverse phase HPLC to yield 2-(3-methyl-4-(pyridazin-4-yl)phenyl)-N-(5-(pyridazin-4-yl)pyridin-2-yl)acetamide 134 as off white solid. MS m/z 383.2 (M+1).

後処理

  1. extractionextracted with 0.5 N HCl solution (30 ml)
  2. extractionThe aqueous extraction
  3. additionwas treated with Na2CO3
  4. extractionfollowed by extraction with ethyl acetate (30 ml×2)
  5. extractionThe combined organic extractions
  6. dry with materialwere dried over Na2SO4
  7. concentrationconcentrated by evaporation

出典と根拠

ORDレコード
ord-5984a87b68904b7bbfecdef5cbc30d0f
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08546396B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート