Triethanolamine → N-(9-oxo-9H-thioxanthene-2-yl)methyl-N,N,N-tris(2-hydroxyethyl)ammonium bromide

HRID 533495

반응식

HRID 533495 반응식
[Br:1][CH2:2][C:3]1[CH:16]=[CH:15][C:14]2[S:13][C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[C:6](=[O:17])[C:5]=2[CH:4]=1.[N:18]([CH2:25][CH2:26][OH:27])([CH2:22][CH2:23][OH:24])[CH2:19][CH2:20][OH:21]>ClCCl>[Br-:1].[O:17]=[C:6]1[C:5]2[CH:4]=[C:3]([CH2:2][N+:18]([CH2:25][CH2:26][OH:27])([CH2:22][CH2:23][OH:24])[CH2:19][CH2:20][OH:21])[CH:16]=[CH:15][C:14]=2[S:13][C:12]2[C:7]1=[CH:8][CH:9]=[CH:10][CH:11]=2

참가 물질

4

반응물 2

HCID 7618TriethanolamineHCID 900012-(bromomethyl)-9H-thioxanthen-9-one

생성물 1

HCID 86666340N-(9-oxo-9H-thioxanthene-2-yl)methyl-N,N,N-tris(2-hydroxyethyl)ammonium bromide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
25 °C

실험 절차

The intermediate (C122-2-2) (2-bromomethylthioxanthone) (1.0 part) was dissolved in dichloromethane (85 g), and triethanol amine [product of Wako Pure Chemical industries, Ltd.] (0.5 parts) was added dropwise to this solution (an exotherm was observed after the addition). The resulting mixture was stirred at room temperature (about 25° C.) for one hour, and the organic solvent was evaporated under reduced pressure. As a result, 2.2 g of white solids were obtained. The white solids were recrystallized in a tetrahydrofuran/dichloromethane mixed solution, and 1.0 part of an intermediate (C122-2-3) was obtained (as brown solids).

후처리

  1. additionafter the addition)
  2. customthe organic solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-1245c93b046441188adfc0390fd784f8
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08853290B2

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