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

HRID 2194863노트

반응식

HRID 2194863 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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%

출처 및 근거

ORD 기록
ord-9fc6e859b1e0452fa7ec827092049ff6
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08334308B2

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