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Acetonitrile → HCID 178479773, 화합물

HRID 1154718
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HRID 1154718 반응식
[Br:1][C:2]1[CH:13]=[CH:12][C:5]2[C:6](=O)[NH:7][S:8](=[O:10])(=[O:9])[C:4]=2[CH:3]=1.P(Cl)(Cl)(Cl)(Cl)[Cl:15].[N:20]1([CH2:26][C:27]2[CH:28]=[C:29]([CH:35]=[CH:36][CH:37]=2)[O:30][CH2:31][CH2:32][CH2:33][NH2:34])[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]1.C(#N)C>ClC1C=CC=CC=1Cl>[ClH:15].[N:20]1([CH2:26][C:27]2[CH:28]=[C:29]([CH:35]=[CH:36][CH:37]=2)[O:30][CH2:31][CH2:32][CH2:33][NH:34][C:6]2[C:5]3[CH:12]=[CH:13][C:2]([Br:1])=[CH:3][C:4]=3[S:8](=[O:10])(=[O:9])[N:7]=2)[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]1
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참가 물질

6

반응물 4

HCID 6342AcetonitrileHCID 24819Phosphorus pentachlorideHCID 102205613-(3-(Piperidin-1-ylmethyl)phenoxy)propan-1-amineHCID 105409966-Bromo-2,3-dihydro-1,2-benzothiazole-1,1,3-trione

생성물 1

HCID 178479773HCID 178479773, 화합물

시약·촉매·용매 1

HCID 7239
1,2-Dichlorobenzene
용매

실험 절차

A mixture of 4.00 g (15 mmol) 6-bromo-1,2-benzisothiazol-3(2H)-one 1,1-dioxide and 3.57 g (17 mmol) phosphorus pentachloride in 5 ml o-dichlorobenzene is heated from ambient temperature to 160° C. over one hour and is held at that temperature for one additional hour. Upon cooling, liquids are removed in vacuo and the residual 6-bromo-3-chlorobenzisothiazole 1,1-dioxide is suspended in acetonitrile and added portionwise to a solution of 3.7 g (15 mmol) 3-[3-[(1-piperidinyl)methyl]phenoxy]propylamine in refluxing acetonitrile. Heating at reflux is continued for one hour after completion of the addition, after which the reaction mixture is cooled to room temperature. The solution is decanted away from a small quantity of gum and the solvent is removed on a rotoevaporator. The resulting oil is dissolved in absolute ethanol, from which the title compound precipitates. m.p. 217°-220° C. IR (KBr) 1625, 1290, 1165, 1150 cm-1

후처리

  1. temperatureis heated from ambient temperature to 160° C. over one hour
  2. temperatureUpon cooling
  3. customliquids are removed in vacuo
  4. temperatureHeating
  5. temperatureat reflux
  6. additionafter completion of the addition
  7. customThe solution is decanted away from a small quantity of gum
  8. customthe solvent is removed on a rotoevaporator
  9. dissolutionThe resulting oil is dissolved in absolute ethanol, from which the title compound
  10. customprecipitates

출처 및 근거

ORD 기록
ord-b995ec928a7a49d3968c51767e759fbb
출처 데이터셋
uspto-grants-1984_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04490527

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