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Acetonitrile → HCID 178479773、化合物

HRID 1154718
ノート
印刷プレビュー

反応式

HRID 1154718 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 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

生成物 1

HCID 178479773HCID 178479773、化合物

試薬・触媒・溶媒 1

HCID 7239
1,2-Dichlorobenzene
溶媒

実験手順

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

後処理

  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

出典と根拠

ORDレコード
ord-b995ec928a7a49d3968c51767e759fbb
出典データセット
uspto-grants-1984_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04490527

反応ノート

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