Methanol → 1,1'-(9,10-Dihydroanthracene-2,6-diyl)bis(2-chloroethanone)

HRID 337389

反応式

HRID 337389 の反応式
[Cl:1][CH2:2][C:3](Cl)=[O:4].[Cl-].[Cl-].[Cl-].[Al+3].[CH:10]1[C:23]2[CH2:22][C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[CH2:15][C:14]=2[CH:13]=[CH:12][CH:11]=1.[CH3:24][OH:25].Cl[CH2:27][Cl:28]>O>[CH:13]1[C:14]2[CH2:15][C:16]3[C:21](=[CH:20][C:19]([C:24](=[O:25])[CH2:27][Cl:28])=[CH:18][CH:17]=3)[CH2:22][C:23]=2[CH:10]=[CH:11][C:12]=1[C:3](=[O:4])[CH2:2][Cl:1]

参加物

7

反応物 5

HCID 887MethanolHCID 6344Dichloromethane2 回HCID 6577Chloroacetyl chlorideHCID 119409,10-DihydroanthraceneHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 867233261,1'-(9,10-Dihydroanthracene-2,6-diyl)bis(2-chloroethanone)

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
-5 °C

実験手順

To a stirred solution of 2-chloroacetyl chloride (3.53 mL, 44.4 mmol) and aluminum trichloride (5.92 g, 44.4 mmol) in dichloromethane (DCM) (50 mL), 9,10-dihydroanthracene (2 g, 11.10 mmol) in dichloromethane (DCM) (50 mL) was added dropwise over 5 min at r.t. and left stirring for 1 h. The reaction mixture was then added to a mixture of methanol (100 mL) and H2O (100 mL) chilled to −5° C. The slurry was warmed to ambient temperature, stirred for 30-60 min. and the solids were collected and were washed well with H2O and dried at 50-60° C. to constant weight.

後処理

  1. waitleft
  2. temperatureThe slurry was warmed to ambient temperature
  3. stirringstirred for 30-60 min.
  4. customthe solids were collected
  5. washwere washed well with H2O
  6. customdried at 50-60° C. to constant weight

出典と根拠

ORDレコード
ord-2803a309e3b9455db086b81d73f5e923
出典データセット
uspto-grants-2014_11
特許番号
US08889726B2

関連ノート

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