Hydrochloric Acid → Diisopropyl Ether

HRID 1282019

반응식

HRID 1282019 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([CH3:12])[C:9]([OH:11])=[O:10])=[CH:4][CH:3]=1.[Cl:13][CH2:14][CH2:15][O:16][C:17](Cl)=[O:18].O.O.O.O.O.O.O.O.O.O.O.O.P([O-])([O-])([O-])=O.[Na+].[Na+].[Na+].Cl.Cl[CH2:42]Cl>>[Cl:13][CH2:14][CH2:15][O:16][C:17]([NH:1][C:2]1[CH:3]=[CH:4][C:5]([CH:8]([CH3:12])[C:9]([OH:11])=[O:10])=[CH:6][CH:7]=1)=[O:18].[CH:15]([O:16][CH:8]([CH3:9])[CH3:12])([CH3:42])[CH3:14]

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 6344DichloromethaneHCID 123052-Chloroethyl chloroformateHCID 430264-Aminohydratropic acidHCID 61473Trisodium phosphate dodecahydrate

생성물 2

HCID 7914Diisopropyl EtherHCID 184235752-(4-{[(2-Chloroethoxy)carbonyl]amino}phenyl)propanoic Acid

실험 절차

1 g (6 mmol) of 2-(4-aminophenyl)propanoic acid was suspended in 30 ml of dichloromethane and 1.24 ml (12 mmol) of 2-chloroethylchloroformate were added at 0° C. under stirring. After 30 minutes at the same temperature 2.27 g (6 mmol) of sodium phosphate dodecahydrate were added portionwise. After 4 hours the reaction was complete (HPLC-MS). The mixture was made acidic by using hydrochloric acid 0.5N and the product extracted with dichloromethane. The organic layer was dried over sodium sulphate and evaporated under vacuum. 1.4 g (100%yield) of the title compound were obtained by crystallization from diisopropylether.

후처리

  1. extractionthe product extracted with dichloromethane
  2. dry with materialThe organic layer was dried over sodium sulphate
  3. customevaporated under vacuum

출처 및 근거

ORD 기록
ord-b8fe52451ece4672826b8d63fb756574
출처 데이터셋
uspto-grants-2002_09
특허 번호
US06455559B1

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