Hydrochloric Acid → 3-Chloro-5-fluoro-4-(hydroxymethyl)phenol

HRID 1772874ノート

反応式

HRID 1772874 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([OH:9])[CH:5]=[C:6]([F:8])[CH:7]=1.[OH-:10].[K+].[CH2:12]=O.Cl>O>[Cl:1][C:2]1[CH:3]=[C:4]([OH:9])[CH:5]=[C:6]([F:8])[C:7]=1[CH2:12][OH:10]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 14797Potassium HydroxideHCID 27737133-Chloro-5-fluorophenol

生成物 1

HCID 222200093-Chloro-5-fluoro-4-(hydroxymethyl)phenol収率 39.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
60 °C

実験手順

3-Chloro-5-fluorophenol (703 mg, 4.8 mmol) was added to a solution of potassium hydroxide (297 mg, 5.3 mmol) in H2O (1.45 mL) and heated at 60° C. Formaldehyde (37 wt % in H2O, 0.74 mL, 9.12 mmol) in H2O (1.45 mL) was added dropwise and the reaction mixture left to stir at 40° C. overnight. The reaction mixture was cooled to rt and conc. HCl (approximately 6 mL) was added. The resultant precipitate was filtered, washed with H2O and dried to yield the title compound as a cream solid (334 mg, 1.89 mmol).

後処理

  1. waitthe reaction mixture left
  2. temperatureThe reaction mixture was cooled to rt
  3. filtrationThe resultant precipitate was filtered
  4. washwashed with H2O
  5. customdried

出典と根拠

ORDレコード
ord-62ff4e8eb3c94d62b31885e78badbe38
出典データセット
uspto-grants-2016_02
特許番号
US09249160B2

反応ノート

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