Water → HCID 19956225、化合物

HRID 1779487ノート

反応式

HRID 1779487 の反応式
P(Cl)(Cl)(Cl)=O.[CH3:6][C:7]1[CH:8]=[CH:9][C:10]([N:16]2[CH:20]=[CH:19][CH:18]=[CH:17]2)=[C:11]([CH:15]=1)[C:12]([OH:14])=O.O>CN(C)C=O>[CH3:6][C:7]1[CH:8]=[CH:9][C:10]2[N:16]3[CH:20]=[CH:19][CH:18]=[C:17]3[C:12](=[O:14])[C:11]=2[CH:15]=1

参加物

5

反応物 3

HCID 962WaterHCID 24813Phosphorus oxychlorideHCID 149135585-Methyl-2-(1H-pyrrol-1-yl)benzoic acid

生成物 1

HCID 19956225HCID 19956225、化合物収率 35%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

At 0° C., add 1.36 ml (14.9 mmol) of phosphorus oxychloride to 1.14 ml (14.9 mmol) of dimethylformamide, then add a solution of 3 g (14.9 mmol) of 5-methyl-2-pyrrol-1-ylbenzoic acid (Preparation 25) in 30 ml of dimethylformamide. After one night's stirring at room temperature, hydrolyse the reaction mixture by pouring into 50 ml of water, extract with 200 ml of diethyl ether, and wash the ethereal phase in succession with water, a saturated aqueous hydrogen carbonate solution and then water. After drying over magnesium sulfate and rendering colourless with animal charcoal, the ethereal phase is concentrated to dryness to yield the title compound.

後処理

  1. extractionextract with 200 ml of diethyl ether
  2. washwash the ethereal phase in succession with water
  3. dry with materialAfter drying over magnesium sulfate and rendering colourless with animal charcoal
  4. concentrationthe ethereal phase is concentrated to dryness

出典と根拠

ORDレコード
ord-386a5f86a788485f86c1969127f186a0
出典データセット
uspto-grants-1997_05
特許番号
US05627203

反応ノート

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