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Sodium hydride → 4-Bromo-1-(2-methoxy-ethoxymethoxy)-2-trifluoromethyl-benzene

HRID 517943
ノート
印刷プレビュー

反応式

HRID 517943 の反応式
[H-].[Na+].[Br:3][C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[C:6]([C:11]([F:14])([F:13])[F:12])[CH:5]=1.Cl[CH2:16][O:17][CH2:18][CH2:19][O:20][CH3:21]>C1COCC1.C(OCC)(=O)C>[Br:3][C:4]1[CH:9]=[CH:8][C:7]([O:10][CH2:16][O:17][CH2:18][CH2:19][O:20][CH3:21])=[C:6]([C:11]([F:12])([F:13])[F:14])[CH:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 24758Sodium hydrideHCID 775901-(Chloromethoxy)-2-methoxyethaneHCID 142784o-Cresol, 4-bromo-alpha,alpha,alpha-trifluoro-

生成物 1

HCID 576575554-Bromo-1-(2-methoxy-ethoxymethoxy)-2-trifluoromethyl-benzene収率 78%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒
HCID 8857
Ethyl Acetate
溶媒

実験手順

Sodium hydride (6.55 g) was added in small portions to a solution of 4-bromo-2-(trifluoromethyl)phenol (32.9 g) in THF (150 ml). After stirring at room temperature for 10 minutes, 1-(chloromethoxy)-2-methoxyethane (17 g) was then added by syringe. The mixture was stirred at room temperature for 24 hours then diluted with ethyl acetate (300 mL) and washed with water. Organics were dried over sodium sulphate and solvent evaporated under reduced pressure. The resulting residue was columned on silica gel using heptane as eluant to afford 4-bromo-1-((2-methoxy-ethoxy)methoxy)-2-(trifluoromethyl)benzene (78% yield).

後処理

  1. stirringThe mixture was stirred at room temperature for 24 hours
  2. washwashed with water
  3. dry with materialOrganics were dried over sodium sulphate and solvent
  4. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-02104602ddbe46f3accfd6231c900024
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09115126B2

反応ノート

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