Dimethylformamide → HCID 1226728、化合物

HRID 1084824ノート

反応式

HRID 1084824 の反応式
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH:6]=[CH:7][C:8]([NH:10][C:11]1[CH:19]=[CH:18][CH:17]=[CH:16][C:12]=1[C:13]([OH:15])=[O:14])=[O:9].[C:20](=O)([O-])[O-].[K+].[K+].CN(C)C=O.CI>CC(C)=O>[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH:6]=[CH:7][C:8]([NH:10][C:11]1[CH:19]=[CH:18][CH:17]=[CH:16][C:12]=1[C:13]([O:15][CH3:20])=[O:14])=[O:9]

参加物

6

反応物 4

HCID 6228Dimethylformamide2 回HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 3063368HCID 3063368、化合物

生成物 1

HCID 1226728HCID 1226728、化合物収率 74.1%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a suspension of 2-[3-(2-thienyl)acrylamido]benzoic acid (273 mg, 1 mmol) in dry acetone (2 ml) were added potassium carbonate (194 mg, 1.4 mmol) and dry dimethylformamide (1 ml). The mixture was treated with methyl iodide (199 mg, 1.4 mmol) and dry dimethylformamide (2 ml) and stirred at room temperature for 3 hours. The reaction mixture was poured into ice water, the precipitated solid was collected on a filter by suction, dried, and recrystallized from the mixed solvent of methanol and water to give pale yellow crystals of the desired compound (213 mg, yield, 74%). m.p., 126°-127° C.

後処理

  1. customthe precipitated solid was collected on
  2. filtrationa filter by suction
  3. customdried
  4. customrecrystallized from the mixed solvent of methanol and water

出典と根拠

ORDレコード
ord-bbf74cbe8e1d4834beecf124acec8e88
出典データセット
uspto-grants-1991_04
特許番号
US05006548

反応ノート

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