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Benzoyl chloride → HCID 15406406、化合物

HRID 616629
ノート
印刷プレビュー

反応式

HRID 616629 の反応式
[C:1]1([C:7]2[C:11]3[CH:12]=[CH:13][C:14]([O:16][CH3:17])=[CH:15][C:10]=3[S:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:18](Cl)(=[O:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.[Cl-].[Al+3].[Cl-].[Cl-]>ClCCCl>[C:18]([C:8]1[S:9][C:10]2[CH:15]=[C:14]([O:16][CH3:17])[CH:13]=[CH:12][C:11]=2[C:7]=1[C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1)(=[O:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7412Benzoyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 15422638HCID 15422638、化合物

生成物 1

HCID 15406406HCID 15406406、化合物収率 52%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

反応条件

温度
0 °C

実験手順

To 100 ml. of 1,2-dichloroethane were added 5.0 g. (0.021 mole) of 3-phenyl-6-methoxybenzothiophene and 2.81 g. (0.021 mole) of benzoyl chloride. The mixture was cooled to 0° C., and 2.93 g. (0.022 mole) of aluminum chloride were added. The mixture was stirred for one hour, and ice then was added. The resulting organic layer was separated, washed with water, and evaporated. To the residue were added 250 ml. of methanol and 10 ml. of 5N sodium hydroxide. The mixture was refluxed for 30 minutes, evaporated, and ether and water were added to the residue. The ether layer was separated, washed with 1N sodium hydroxide, 1N hydrochloric acid, and aqueous soidum chloride. The ether layer then was dried over magnesium sulfate, filtered, and evaporated. The residue was crystallized from methanol to obtain 3.77 g. (52 percent) of the title compound, m.p. 94°-95.5° C.

後処理

  1. additionice then was added
  2. customThe resulting organic layer was separated
  3. washwashed with water
  4. customevaporated
  5. additionTo the residue were added 250 ml
  6. temperatureThe mixture was refluxed for 30 minutes
  7. customevaporated
  8. additionether and water were added to the residue
  9. customThe ether layer was separated
  10. washwashed with 1N sodium hydroxide, 1N hydrochloric acid, and aqueous soidum chloride
  11. dry with materialThe ether layer then was dried over magnesium sulfate
  12. filtrationfiltered
  13. customevaporated
  14. customThe residue was crystallized from methanol
  15. customto obtain 3.77 g

出典と根拠

ORDレコード
ord-8cad5b6157cb43d79cbec7d1ab51a421
出典データセット
uspto-grants-1978_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04075227

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート