5-Fluorobenzene-1,3-diol → Umbelliferone

HRID 253720

반응식

HRID 253720 반응식
F[C:2]1[CH:7]=[C:6]([OH:8])[CH:5]=[C:4]([OH:9])[CH:3]=1>S(=O)(=O)(O)O>[OH:9][C:4]1[CH:5]=[C:6]2[C:7]([CH:4]=[CH:5][C:6](=[O:8])[O:8]2)=[CH:2][CH:3]=1

참가 물질

3

반응물 1

HCID 126587785-Fluorobenzene-1,3-diol

생성물 1

HCID 5281426Umbelliferone수율 146.9%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

1-Fluoro-3,5-dihydroxybenzene (1.0 g, 7.8 mmol) and ethyl 2-benzyl acetoacetate (1.72 g, 7.8 mmol) are suspended in 20 mL of 70% sulfuric acid at room temperature. The reaction mixture is stirred for 24 hours and poured into ice water. The solid is filtered and washed with water. The yellowish crude product is re-crystallized from hot ethanol to afford the 7-hydroxy coumarin intermediate (929 mg, 42%).

후처리

  1. filtrationThe solid is filtered
  2. washwashed with water
  3. customThe yellowish crude product is re-crystallized from hot ethanol

출처 및 근거

ORD 기록
ord-6b3dab5e691549ec9674ed348d6cad28
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07872142B2

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