HCID 20303506、化合物 → 4-Amino-2,5-dichloro-α-methylbenzeneacetic acid

HRID 1733007ノート

反応式

HRID 1733007 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([N+:8]([O-])=O)[C:5]([Cl:11])=[CH:4][C:3]=1[CH:12]([CH3:16])[C:13]([OH:15])=[O:14]>C(O)(=O)C.O.[Fe]>[NH2:8][C:6]1[C:5]([Cl:11])=[CH:4][C:3]([CH:12]([CH3:16])[C:13]([OH:15])=[O:14])=[C:2]([Cl:1])[CH:7]=1

参加物

5

反応物 1

HCID 20303506HCID 20303506、化合物

生成物 1

HCID 203035654-Amino-2,5-dichloro-α-methylbenzeneacetic acid収率 78.6%

試薬・触媒・溶媒 3

HCID 23925Iron触媒HCID 176Acetic Acid溶媒HCID 962Water溶媒

反応条件

温度
95 °C

実験手順

23 g (87 mmoles) of 2-(2,5-dichloro-4-nitrophenyl)propionic acid are heated to 95° C. in 100 ml of glacial acetic acid and 30 ml of water, and 14 g (0.25 mole) of iron powder are added in portions. After the exothermic reaction subsides, heating (to 95° C.) is effected for a further hour. Pouring onto 500 g of ice is effected, followed by extracting twice with, in each case, 200 ml of diethyl ether, washing the organic phase with water, drying, and concentrating in a vacuum to obtain 16 g (78.6% of theory) of 2-(4-amino-2,5-dichlorophenyl)propionic acid (m.p. 140° to 141° C.).

後処理

  1. customAfter the exothermic reaction subsides
  2. waitis effected for a further hour
  3. extractionby extracting twice with, in each case, 200 ml of diethyl ether
  4. washwashing the organic phase with water
  5. customdrying
  6. concentrationconcentrating in a vacuum

出典と根拠

ORDレコード
ord-7ade05bc802145e1b10e5627d2c9638c
出典データセット
uspto-grants-1980_12
特許番号
US04239901

反応ノート

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