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

HRID 72283노트

반응식

HRID 72283 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매2회

반응 조건

온도
60 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-88d86efd347a4ea9ad9cf8574adee841
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08828908B2

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