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

HRID 1485332ノート

反応式

HRID 1485332 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 μmol) 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-chlorohexyloxy)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-3bd4000dabc24177a8253d649e5c5f77
出典データセット
uspto-grants-2016_08
特許番号
US09422294B2

反応ノート

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