Thionyl Chloride → 3,5-Diamino-2-methylbenzoic acid

HRID 19970

反応式

HRID 19970 の反応式
S(Cl)(Cl)=O.[NH2:5][C:6]1[CH:7]=[C:8]([CH:12]=[CH:13][C:14]=1[NH2:15])[C:9]([OH:11])=[O:10].[C:16](=O)(O)[O-].[Na+]>CO>[CH3:16][O:10][C:9](=[O:11])[C:8]1[CH:12]=[CH:13][C:14]([NH2:15])=[C:6]([NH2:5])[CH:7]=1

参加物

5

反応物 3

HCID 24386Thionyl ChlorideHCID 692633,4-Diaminobenzoic acidHCID 516892Sodium Bicarbonate

生成物 1

HCID 1355243,5-Diamino-2-methylbenzoic acid収率 81%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To dry methanol (20 ml) was carefully added thionyl chloride (1 ml) dropwise with stirring. The 3,4-diaminobenzoic acid (1 g) was added in portions at R.T. with stirring then the mixture heated at reflux for 3 h. Saturated sodium bicarbonate was added until the mixture was basic, then the mixture extracted into chloroform containing 25% methanol. The extract was dried and evaporated in vacuo to give the product (0.88 g, 81%) as a brown crystalline solid.

後処理

  1. stirringwith stirring
  2. temperaturethe mixture heated
  3. temperatureat reflux for 3 h
  4. extractionthe mixture extracted into chloroform containing 25% methanol
  5. customThe extract was dried
  6. customevaporated in vacuo

出典と根拠

ORDレコード
ord-79f45971a6444b508008851ae0cf9325
出典データセット
uspto-grants-2010_06
特許番号
US07745490B2

関連ノート

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