Hydrochloric Acid → 2-Fluoro-3-iodo-4-methoxybenzaldehyde

HRID 2212590ノート

反応式

HRID 2212590 の反応式
[F:1][C:2]1[C:7]([I:8])=[C:6]([O:9][CH3:10])[CH:5]=[CH:4][C:3]=1[CH:11]1OCC[O:12]1.Cl>CC(C)=O>[F:1][C:2]1[C:7]([I:8])=[C:6]([O:9][CH3:10])[CH:5]=[CH:4][C:3]=1[CH:11]=[O:12]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 219664342-(2-Fluoro-3-iodo-4-methoxy-phenyl)-[1,3] dioxolane

生成物 1

HCID 219664772-Fluoro-3-iodo-4-methoxybenzaldehyde収率 48.6%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a solution of 2-(2-fluoro-3-iodo-4-methoxy-phenyl)-[1,3] dioxolane (5.284 g, 16.30 mmol) in acetone (170 mL) was added HCl (1N, 170 mL) and the solution stirred at room temperature for 48 hrs. The solution was extracted with ethyl acetate and washed successively with water, brine, dried (MgSO4), filtered and evaporated. The residue was purified on silica gel (eluent: 10% ethyl acetate in hexane) to give 2.22 g of 2-Fluoro-3-iodo-4-methoxy benzaldehyde (38% for 2 steps). 1H NMR (300 MHz; CDCl3): 4.00 (s, 3 H), 6.74 (d, J=8.4 Hz, 1 H), 7.88 (t, J=8.1 Hz, 1 H), 10.21 (s, 1 H).

後処理

  1. extractionThe solution was extracted with ethyl acetate
  2. washwashed successively with water, brine
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue was purified on silica gel (eluent: 10% ethyl acetate in hexane)

出典と根拠

ORDレコード
ord-c29e27536d2b4a968de576fb71c65369
出典データセット
uspto-grants-2006_09
特許番号
US07102000B2

反応ノート

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