Trimethyl orthoformate → HCID 66985986、化合物

HRID 2069932ノート

反応式

HRID 2069932 の反応式
[Br:1][C:2]1[C:3]([O:10][CH3:11])=[C:4]([CH:7]=[CH:8][CH:9]=1)C=O.CO[CH:14]([O:17][CH3:18])[O:15][CH3:16].ClS(O)(=O)=O>CO>[Br:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:4]([CH:14]([O:15][CH3:16])[O:17][CH3:18])[C:3]=1[O:10][CH3:11]

参加物

5

反応物 3

HCID 9005Trimethyl orthoformateHCID 24638Chlorosulfonic acidHCID 110638083-Bromo-2-methoxybenzaldehyde

生成物 1

HCID 66985986HCID 66985986、化合物収率 81%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

3-Bromo-2-methoxybenzaldehyde (28 g, 130 mmol) was combined with trimethylorthoformate (27.5 g, 28.6 mL, 260 mmol) in methanol (150 mL) and then chlorosulfonic acid (0.5 mL) was added dropwise to the mixture. The mixture was stirred for 3 hours and then concentrated by rotoevaporation. The residue was partitioned between ethyl ether and 5% aqueous sodium bicarbonate and the organic layer was separated, washed with water and brine, dried over sodium sulfate and concentrated to give 1-bromo-3-dimethoxymethyl-2-methoxybenzene (27.5 g).

後処理

  1. concentrationconcentrated by rotoevaporation
  2. customThe residue was partitioned between ethyl ether and 5% aqueous sodium bicarbonate
  3. customthe organic layer was separated
  4. washwashed with water and brine
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-ae096e5774284027bd8baaac623d7419
出典データセット
uspto-grants-2012_10
特許番号
US08299110B2

反応ノート

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