Ethyl Acetate → HCID 67412867、化合物

HRID 910169ノート

反応式

HRID 910169 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8](=[N:14][N:15]([CH3:17])[CH3:16])[N:9]1[CH:13]=[CH:12][N:11]=[CH:10]1.Cl[CH2:19][O:20][C:21]1[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][CH:22]=1.C(=O)([O-])[O-].[K+].[K+].C(OCC)(=O)C>CN(C)C=O>[Cl:27][C:24]1[CH:25]=[CH:26][C:21]([O:20][CH2:19][O:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=2[C:8](=[N:14][N:15]([CH3:17])[CH3:16])[N:9]2[CH:13]=[CH:12][N:11]=[CH:10]2)=[CH:22][CH:23]=1

参加物

6

反応物 4

HCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 88801alpha,4-DichloroanisoleHCID 136337079HCID 136337079、化合物

生成物 1

HCID 67412867HCID 67412867、化合物収率 63%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of the Compound No. 13 (0.20 g, 0.869 mmol) obtained in Example 13 in N,N-dimethylformamide (3 ml) were added α,4-dichloroanisole (0.175 g, 0.989 mmol) and potassium carbonate (0.17 g, 1.23 mmol), and the mixture was stirred at room temperature for 20 hr. Ethyl acetate was added to the reaction mixture, the mixture was washed with water, and the organic layer was dried over sodium sulfate. The solvent was evaporated under reduced pressure, and the obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate) to give the object compound (0.202 g, 0.545 mmol, yield 63%).

後処理

  1. washthe mixture was washed with water
  2. dry with materialthe organic layer was dried over sodium sulfate
  3. customThe solvent was evaporated under reduced pressure
  4. customthe obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate)

出典と根拠

ORDレコード
ord-8b743c0133bf40f388a5503170bd1cec
出典データセット
uspto-grants-2011_09
特許番号
US08022072B2

反応ノート

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