4-Methylmorpholine → HCID 67050039、化合物

HRID 217631

反応式

HRID 217631 の反応式
CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[NH2:25][C:26]1[C:30]([NH:31][C:32]([O:34][C:35]([CH3:38])([CH3:37])[CH3:36])=[O:33])=[CH:29][S:28][CH:27]=1.[CH3:39][O:40][C:41]([C:43]1[CH:44]=[CH:45][C:46]([C:49](O)=[O:50])=[N:47][CH:48]=1)=[O:42].CN1CCOCC1>CN(C=O)C.C(OCC)(=O)C.O>[C:35]([O:34][C:32]([NH:31][C:30]1[C:26]([NH:25][C:49]([C:46]2[CH:45]=[CH:44][C:43]([C:41]([O:40][CH3:39])=[O:42])=[CH:48][N:47]=2)=[O:50])=[CH:27][S:28][CH:29]=1)=[O:33])([CH3:38])([CH3:37])[CH3:36]

参加物

8

反応物 4

HCID 79724-MethylmorpholineHCID 3149925-(Methoxycarbonyl)pyridine-2-carboxylic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 11063797HCID 11063797、化合物

生成物 1

HCID 67050039HCID 67050039、化合物収率 67%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

HATU (1.3 g, 3.5 mmol) was added to a solution of 3-amino-4-t-butoxycarbonylaminothiophene (Reference Compound No. 1-1, 0.68 g, 3.2 mmol), 5-methoxycarbonylpyridine-2-carboxylic acid (0.64 g, 3.5 mmol), and N-methylmorpholine (0.70 mL, 6.4 mmol) in DMF (20 mL), and then the reaction mixture was stirred at room temperature overnight. Water (0.30 L) and ethyl acetate (0.40 L) were added thereto, and the insoluble materials were filtered off to give 0.50 g of the title reference compound as a pale yellow solid. The filtrate was partitioned and the organic layer was dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and then the obtained solid was collected by filtration with ethylacetate (30 mL) to give 0.30 g of the title reference compound as a pale brown solid. (Yield 67%)

後処理

  1. filtrationthe insoluble materials were filtered off
  2. customto give 0.50 g of the title reference compound as a pale yellow solid
  3. customThe filtrate was partitioned
  4. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. filtrationthe obtained solid was collected by filtration with ethylacetate (30 mL)
  7. customto give 0.30 g of the title reference compound as a pale brown solid

出典と根拠

ORDレコード
ord-10d61d39493341c88cd84f7b81bfdad3
出典データセット
uspto-grants-2012_06
特許番号
US08198271B2

関連ノート

読み込み中…