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Water → 1-Benzyl-4-benzylamino-6-trifluoromethyl-1,3-dihydro-imidazo[4,5-c]pyridine-2-one

HRID 639620
ノート
印刷プレビュー

反応式

HRID 639620 の反応式
[CH2:1]([NH:8][C:9]1[C:14]([NH2:15])=[C:13]([NH:16][CH2:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:12]=[C:11]([C:24]([F:27])([F:26])[F:25])[N:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.CCCCCCC.C[CH2:37][O:38]C(C)=O>CC(OC)(C)C>[CH2:17]([N:16]1[C:13]2[CH:12]=[C:11]([C:24]([F:27])([F:26])[F:25])[N:10]=[C:9]([NH:8][CH2:1][C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)[C:14]=2[NH:15][C:37]1=[O:38])[C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 8900HeptaneHCID 67456850N2,N4-Dibenzyl-6-trifluoromethyl-pyridine-2,3,4-triamine

生成物 1

HCID 674571721-Benzyl-4-benzylamino-6-trifluoromethyl-1,3-dihydro-imidazo[4,5-c]pyridine-2-one

試薬・触媒・溶媒 1

HCID 15413tert-Butyl methyl ether
溶媒

実験手順

N2,N4-Dibenzyl-6-trifluoromethyl-pyridine-2,3,4-triamine (9.02 g, 24.2 mmol) was dissolved in TBME (180 ml) and CDl (19.6 g, 121 mmol) was added. The reaction mixture was stirred at room temperature for 72 h. Water (100 ml) was added to the reaction mixture and the layers were separated. The aqueous was extracted with EtOAc (200 ml). The combined organics were washed with brine (50 ml), dried over MgSO4 and concentrated in vacuo to give the crude (25 g). Column chromatography through silica eluting with 30:70→60:40 Heptane:EtOAc gave the title compound (2.64 g) as a white fluffy solid.

後処理

  1. additionCDl (19.6 g, 121 mmol) was added
  2. customthe layers were separated
  3. extractionThe aqueous was extracted with EtOAc (200 ml)
  4. washThe combined organics were washed with brine (50 ml)
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated in vacuo
  7. customto give the crude (25 g)

出典と根拠

ORDレコード
ord-b849caf7a44f4062a02a0d098c8f39da
出典データセット
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07691877B2

反応ノート

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