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HCID 19838166、化合物 → HCID 22750172、化合物

HRID 2083694
ノート
印刷プレビュー

反応式

HRID 2083694 の反応式
[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([CH2:23][CH2:24][NH:25][CH2:26][C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[CH:12]=[CH:13][C:14]=1[O:15][CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[S:33]([C:37]1[CH:46]=[CH:45][C:40]([O:41][CH2:42][CH2:43][Cl:44])=[CH:39][CH:38]=1)(=[O:36])(=[O:35])[NH2:34]>C1(C)C(C)=CC=CC=1>[ClH:44].[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([CH2:23][CH2:24][N:25]([CH2:26][C:27]2[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=2)[CH2:43][CH2:42][O:41][C:40]2[CH:39]=[CH:38][C:37]([S:33](=[O:36])(=[O:35])[NH2:34])=[CH:46][CH:45]=2)[CH:12]=[CH:13][C:14]=1[O:15][CH2:16][C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 19838166HCID 19838166、化合物HCID 221651544-(2-Chloroethoxy)benzene-1-sulfonamide

生成物 1

HCID 22750172HCID 22750172、化合物収率 43.2%

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

A mixture of N-2-(3,4-dibenzyloxyphenyl)ethyl benzylamine (13.6 g.), 2-(4-sulfamoylphenoxy)ethyl chloride (4.8 g.) and dry xylene (50 ml.) was boiled under reflux for 12 hours. The solution was cooled and the precipitated solid removed by filtration, the filtrate then being evaporated in vacuo to dryness and taken up into diethyl ether. Insoluble material was removed from the ethereal solution by filtration, and the filtrate treated with ethereal hydrogen chloride, which resulted in the precipitation of a yellow solid. The latter was collected by filtration and recrystallized from a methanol/isopropanol mixture giving N-[2-(3,4-dibenzyloxyphenyl)ethyl]-N-[2-(4-sulfamoylphenoxy) ethyl] benzylamine hydrochloride (5.8 g.), m.p. 178°-181° C.

後処理

  1. temperatureunder reflux for 12 hours
  2. temperatureThe solution was cooled
  3. customthe precipitated solid removed by filtration
  4. customthe filtrate then being evaporated in vacuo to dryness
  5. customInsoluble material was removed from the ethereal solution by filtration
  6. additionthe filtrate treated with ethereal hydrogen chloride, which
  7. customresulted in the precipitation of a yellow solid
  8. filtrationThe latter was collected by filtration
  9. customrecrystallized from a methanol/isopropanol mixture

出典と根拠

ORDレコード
ord-da8442df88094fa4a2e8b5b54b6af4de
出典データセット
uspto-grants-1978_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04086272

反応ノート

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