Hydrochloric Acid → Diisopropyl Ether

HRID 1282019

反応式

HRID 1282019 の反応式
[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]

参加物

7

反応物 5

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

生成物 2

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

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-b8fe52451ece4672826b8d63fb756574
出典データセット
uspto-grants-2002_09
特許番号
US06455559B1

関連ノート

読み込み中…