Hydrochloric Acid → 4'-Chloro-3,5-diethylbiphen-4-ylamine

HRID 72283ノート

反応式

HRID 72283 の反応式
Cl.C(OC(=O)[NH:8][C:9]1[C:14]([CH2:15][CH3:16])=[CH:13][C:12]([C:17]2[CH:22]=[CH:21][C:20]([Cl:23])=[CH:19][CH:18]=2)=[CH:11][C:10]=1[CH2:24][CH3:25])(C)(C)C>CO>[Cl:23][C:20]1[CH:21]=[CH:22][C:17]([C:12]2[CH:11]=[C:10]([CH2:24][CH3:25])[C:9]([NH2:8])=[C:14]([CH2:15][CH3:16])[CH:13]=2)=[CH:18][CH:19]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 59450514(4'-Chloro-3,5-diethylbiphen-4-yl)carbamic acid tert-butyl ester

生成物 1

HCID 594504894'-Chloro-3,5-diethylbiphen-4-ylamine収率 61.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

反応条件

温度
60 °C

実験手順

Concentrated hydrochloric acid (22 ml) is added to a solution of (4′-chloro-3,5-diethylbiphen-4-yl)carbamic acid tert-butyl ester (22 g, 0.06 mol) in methanol (110 ml), and the reaction mixture is heated to 60° C. for 2 hours. The mixture is cooled to room temperature and most of the methanol is removed by evaporation under reduced pressure. The mixture is diluted with water, made basic by addition of 2N aqueous potassium hydroxide solution and extracted with ethyl acetate (3×200 ml). The organic extracts are combined and the solvents are removed under reduced pressure to give 4′-chloro-3,5-diethylbiphen-4-ylamine (9.6 g).

後処理

  1. customis removed by evaporation under reduced pressure
  2. additionThe mixture is diluted with water
  3. additionmade basic by addition of 2N aqueous potassium hydroxide solution
  4. extractionextracted with ethyl acetate (3×200 ml)
  5. customthe solvents are removed under reduced pressure

出典と根拠

ORDレコード
ord-88d86efd347a4ea9ad9cf8574adee841
出典データセット
uspto-grants-2014_09
特許番号
US08828908B2

反応ノート

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