Potassium Carbonate → HCID 67465591、化合物

HRID 2171184ノート

反応式

HRID 2171184 の反応式
[Br:1][C:2]1[C:3]([O:11][CH2:12][O:13][CH3:14])=[C:4]([OH:10])[C:5]([O:8][CH3:9])=[CH:6][CH:7]=1.C(=O)([O-])[O-].[K+].[K+].[CH:21]1([CH2:24]Br)[CH2:23][CH2:22]1>C(#N)C>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[C:4]([O:10][CH2:24][CH:21]2[CH2:23][CH2:22]2)[C:3]=1[O:11][CH2:12][O:13][CH3:14]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 81503BromomethylcyclopropaneHCID 67466846HCID 67466846、化合物

生成物 1

HCID 67465591HCID 67465591、化合物収率 38.5%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a stirring solution of 3-bromo-6-methoxy-2-(methoxymethoxy)phenol (12 g, 0.045 mol) in acetonitrile (100 mL) at 0° C. was added potassium carbonate (18 g, 0.135 mol) and cyclopropylmethyl bromide (9 g, 0.067 mol) and the resultant reaction mixture was stirred for 1 h at RT. The reaction mixture was filtered through celite and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography (silica gel, 0-12% ethyl acetate in pet ether) to afford 1-Bromo-3-(cyclopropylmethoxy)-4-methoxy-2-(methoxymethoxy)benzene as a solid (5.5 g, 38%).

後処理

  1. customthe resultant reaction mixture
  2. filtrationThe reaction mixture was filtered through celite
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe residue was purified by column chromatography (silica gel, 0-12% ethyl acetate in pet ether)

出典と根拠

ORDレコード
ord-c5257943ab174d788140b7b57606f356
出典データセット
uspto-grants-2015_06
特許番号
US09051290B2

反応ノート

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