Acetic Acid → 1-(Chloromethyl)-4-fluoronaphthalene

HRID 8205

反応式

HRID 8205 の反応式
[F:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[CH:4][CH:3]=1.C=O.P(=O)(O)(O)O.[ClH:19].[C:20](O)(=O)C>O>[Cl:19][CH2:20][C:5]1[C:6]2[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=2)[C:2]([F:1])=[CH:3][CH:4]=1

参加物

7

反応物 5

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 1004Phosphoric AcidHCID 94501-Fluoronaphthalene

生成物 1

HCID 156574171-(Chloromethyl)-4-fluoronaphthalene

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 1-fluoronaphthalene (5.5 g, 37.6 mmol), paraformaldehyde (2.5 g, 83 mmol), glacial acetic acid (3.5 mL), phosphoric acid (2 mL) and concentrated hydrochloric acid (5 mL) is heated at 85° C. for 15 h. The reaction mixture is poured into water and extracted three times with dichloromethane. The organic extracts are combined and washed with water and brine, dried (sodium sulfate), filtered, and evaporated to yield the title compound, 6.53 g (98%, as a yellow solid.

後処理

  1. extractionextracted three times with dichloromethane
  2. washwashed with water and brine
  3. dry with materialdried (sodium sulfate)
  4. filtrationfiltered
  5. customevaporated

出典と根拠

ORDレコード
ord-eb6b605148f94f1c8e3a24b3c564aca0
出典データセット
uspto-grants-2006_08
特許番号
US07087626B2

関連ノート

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