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Benzene → HCID 13656356、化合物

HRID 979722
ノート
印刷プレビュー

反応式

HRID 979722 の反応式
C1C=CC=CC=1.[C:7]([C:11]1[CH:12]=[C:13]([OH:18])[CH:14]=[CH:15][C:16]=1[Cl:17])([CH3:10])([CH3:9])[CH3:8].[Cl:19][C:20](OC(Cl)(Cl)Cl)=[O:21].C(N(CC)CC)C>CCCCCC>[Cl:19][C:20]([O:18][C:13]1[CH:14]=[CH:15][C:16]([Cl:17])=[C:11]([C:7]([CH3:10])([CH3:8])[CH3:9])[CH:12]=1)=[O:21]
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 241Benzene2 回HCID 8471TriethylamineHCID 10426DiphosgeneHCID 109102303-Tert-butyl-4-chlorophenol

生成物 1

HCID 13656356HCID 13656356、化合物収率 135.7%

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

Into 50 ml of benzene were dissolved 9.2 g of 3-tert-butyl-4-chlorophenol and 5.5 g of trichloromethyl chloroformate, and a solution obtained by dissolving 5.8 g of triethylamine into 20 ml of benzene was added dropwise thereto with stirring and cooling by ice. After completion of this dropwise addition, the mixture was subjected to stirring for 12 hours at room temperature. To the reaction mixture were added 70 ml of hexane, and precipitated crystal was separated by filtration. The filtrate was washed with water and a saturated aqueous solution of sodium chloride in this order, and was dried over anhydrous calcium chloride. Thereafter, solvent was distilled off. The residue was distilled under reduced pressure to give 9.32 g of 3-tert-butyl-4-chlorophenyl chloroformate having boiling point of 105°-108° C./1 mmHg, of which properties are as follows.

後処理

  1. customa solution obtained
  2. additionwas added dropwise
  3. temperaturecooling by ice
  4. additionAfter completion of this dropwise addition
  5. stirringto stirring for 12 hours at room temperature
  6. customprecipitated crystal
  7. customwas separated by filtration
  8. washThe filtrate was washed with water
  9. dry with materiala saturated aqueous solution of sodium chloride in this order, and was dried over anhydrous calcium chloride
  10. distillationThereafter, solvent was distilled off
  11. distillationThe residue was distilled under reduced pressure

出典と根拠

ORDレコード
ord-fd2589d8df3543cd933ac121e183c8a2
出典データセット
uspto-grants-1987_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04668831

反応ノート

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