Bromotrimethylsilane → 1,3-Dichloro-2-{2-[4-(bromomethyl)phenoxy]ethoxy}-5-methylbenzene

HRID 2194863ノート

反応式

HRID 2194863 の反応式
[Cl:1][C:2]1[CH:19]=[C:18]([CH3:20])[CH:17]=[C:16]([Cl:21])[C:3]=1[O:4][CH2:5][CH2:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14]O)=[CH:10][CH:9]=1.C[Si]([Br:26])(C)C>C(Cl)Cl>[Cl:1][C:2]1[CH:19]=[C:18]([CH3:20])[CH:17]=[C:16]([Cl:21])[C:3]=1[O:4][CH2:5][CH2:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14][Br:26])=[CH:10][CH:9]=1

参加物

4

反応物 2

HCID 76113BromotrimethylsilaneHCID 67447508{4-[2-(2,6-Dichloro-4-methylphenoxy)ethoxy]phenyl}methanol

生成物 1

HCID 584884381,3-Dichloro-2-{2-[4-(bromomethyl)phenoxy]ethoxy}-5-methylbenzene

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of {4-[2-(2,6-dichloro-4-methylphenoxy)ethoxy]phenyl}methanol from II.1, step 3 (1 eq.) in CH2Cl2 (0.1M) at room temperature was added a solution of trimethyl silyl bromide (1.05 eq.) in CH2Cl2 (1.0M). The final mixture was stirred 1 h at room temperature and then concentrated in vacuo. To the resulting suspension was added silica gel and the mixture was evaporated in vacuo. Purification by column chromatography on silica gel, eluting with Hex/Et2O 5%, afforded the desired compound as a crystalline white solid.

後処理

  1. concentrationconcentrated in vacuo
  2. additionTo the resulting suspension was added silica gel
  3. customthe mixture was evaporated in vacuo
  4. customPurification by column chromatography on silica gel
  5. washeluting with Hex/Et2O 5%

出典と根拠

ORDレコード
ord-9fc6e859b1e0452fa7ec827092049ff6
出典データセット
uspto-grants-2012_12
特許番号
US08334308B2

反応ノート

読み込み中…