Potassium Carbonate → 2-(2-Chloro-5-(2-methoxyethoxy)phenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane

HRID 1094816

反応式

HRID 1094816 の反応式
[CH3:1][O:2][CH2:3][CH2:4]OS(C)(=O)=O.[Cl:10][C:11]1[CH:16]=[CH:15][C:14]([OH:17])=[CH:13][C:12]=1[B:18]1[O:22][C:21]([CH3:24])([CH3:23])[C:20]([CH3:26])([CH3:25])[O:19]1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C(=O)C>[Cl:10][C:11]1[CH:16]=[CH:15][C:14]([O:17][CH2:4][CH2:3][O:2][CH3:1])=[CH:13][C:12]=1[B:18]1[O:22][C:21]([CH3:24])([CH3:23])[C:20]([CH3:26])([CH3:25])[O:19]1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 1462932-Methoxyethyl methanesulfonateHCID 534868364-Chloro-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenol

生成物 1

HCID 575823372-(2-Chloro-5-(2-methoxyethoxy)phenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

Methanesulfonic acid 2-methoxyethyl ester (70.5 mg, 0.50 mmol) and 2-[2-chloro-5-hydroxyphenyl]-4,4,5,5-tetramethyl-[1,3,2]-dioxaborolane (Preparation 66,100 mg, 0.42 mmol) were stirred together in N,N-dimethylacetamide (4 ml). Potassium carbonate (58 mg, 0.42 mmol) was added and the resultant solution was heated to 100° C. for 10 hours. The reaction mixture was cooled then quenched with water (10 ml) and extracted with ethylacetate (10 ml). The organic layer was dried over anhydrous MgSO4 (s), filtered and evaporated in vacuo to give crude title compound. Material taken on without further purification.

後処理

  1. temperatureThe reaction mixture was cooled
  2. customthen quenched with water (10 ml)
  3. extractionextracted with ethylacetate (10 ml)
  4. dry with materialThe organic layer was dried over anhydrous MgSO4 (s)
  5. filtrationfiltered
  6. customevaporated in vacuo

出典と根拠

ORDレコード
ord-23207f8d35724c8bb5b85572a84a2b42
出典データセット
uspto-grants-2012_03
特許番号
US08134007B2

関連ノート

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