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

HRID 1772874노트

반응식

HRID 1772874 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
60 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-62ff4e8eb3c94d62b31885e78badbe38
출처 데이터셋
uspto-grants-2016_02
특허 번호
US09249160B2

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