Trifluoroacetic acid → 2-[2-(6-Chlorohexyloxy)ethoxy]ethylammonium trifluoroacetate

HRID 1397968ノート

反応式

HRID 1397968 の反応式
[Cl:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][O:8][CH2:9][CH2:10][O:11][CH2:12][CH2:13][NH:14]C(=O)OC(C)(C)C.[F:22][C:23]([F:28])([F:27])[C:24]([OH:26])=[O:25].ClCCl.CO>ClCCl>[F:22][C:23]([F:28])([F:27])[C:24]([O-:26])=[O:25].[Cl:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][O:8][CH2:9][CH2:10][O:11][CH2:12][CH2:13][NH3+:14]

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 21226129Dichloromethane methanolHCID 52953440tert-Butyl (2-(2-((6-chlorohexyl)oxy)ethoxy)ethyl)carbamate2 回

生成物 1

HCID 866717092-[2-(6-Chlorohexyloxy)ethoxy]ethylammonium trifluoroacetate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

Under argon atmosphere, to a solution of tert-butyl N-[2-{2-(6-chlorohexyloxy)ethoxy}ethyl]carbamate (11) (synthesized by the method described in Non-Patent Document Y. Zhang, M.-k. So, A. M. Loening, H. Yao, S. S. Gambhir, J. Rao, Angew. Chem. Int. Ed., 2006, 118, 4936-4940) (84.2 mg, 260 pump in dichloromethane (2.5 mL) was added trifluoroacetic acid (0.5 mL) at 0° C. After stirring for 2 hours at the same temperature of 0° C., the starting compound 11 completely disappeared as judged from TLC study (Rf=0.41, dichloromethane/methanol=9/1). The reaction solution was then concentrated under reduced pressure using an evaporator to give crude 2-[2-(6-chloro hexyloxy)ethoxy]ethylammonium trifluoroacetate (12) as a colorless oil. The crude product was used in the next reaction without further purification.

後処理

  1. concentrationThe reaction solution was then concentrated under reduced pressure
  2. customan evaporator

出典と根拠

ORDレコード
ord-5ded7405e92c4027b150a23d4a9306c5
出典データセット
uspto-grants-2014_12
特許番号
US08901312B2

反応ノート

読み込み中…