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o-Phenetidine → 2-(2-Ethoxyanilino)methyl-4-propylmorpholine toluene-p-sulphonate

HRID 1283101
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HRID 1283101 반응식
[CH2:1]([O:3][C:4]1[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=1[NH2:6])[CH3:2].[CH2:11]([N:14]1[CH2:19][CH2:18][O:17][CH:16]([CH2:20][O:21][S:22]([C:25]2[CH:30]=[CH:29][C:28]([CH3:31])=[CH:27][CH:26]=2)(=[O:24])=[O:23])[CH2:15]1)[CH2:12][CH3:13]>C1(C)C(C)=CC=CC=1>[C:28]1([CH3:31])[CH:27]=[CH:26][C:25]([S:22]([OH:24])(=[O:21])=[O:23])=[CH:30][CH:29]=1.[CH2:1]([O:3][C:4]1[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=1[NH:6][CH2:20][CH:16]1[O:17][CH2:18][CH2:19][N:14]([CH2:11][CH2:12][CH3:13])[CH2:15]1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 7203o-PhenetidineHCID 214303624-n-Propyl-2-toluene-p-sulphonyloxymethylmorpholine

생성물 1

HCID 215192902-(2-Ethoxyanilino)methyl-4-propylmorpholine toluene-p-sulphonate

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

A solution of 2-ethoxyaniline (4.8 g.) and 4-n-propyl-2-toluene-p-sulphonyloxymethylmorpholine (10 g.) in xylene (50 ml.) is heated under reflux in an atmosphere of nitrogen for 60 hours. A resinous solid separates from the solvent which is distilled under reduced pressure. The residual sticky solid is washed with ether to give a yellow solid which is crystallised from methanol/ether to give 2-(2-ethoxyanilino)methyl-4-propylmorpholine toluene-p-sulphonate, m.p. 169°-172°C.

후처리

  1. temperatureunder reflux in an atmosphere of nitrogen for 60 hours
  2. distillationA resinous solid separates from the solvent which is distilled under reduced pressure
  3. washThe residual sticky solid is washed with ether
  4. customto give a yellow solid which
  5. customis crystallised from methanol/ether

출처 및 근거

ORD 기록
ord-aba26f2c82b34e1e9d68b35ada05950b
출처 데이터셋
uspto-grants-1976_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03974158

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