Water → 3-(Methylsulfonyloxy)phenylboronic acid

HRID 216934

反応式

HRID 216934 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([B:8]([OH:10])[OH:9])[CH:5]=[CH:6][CH:7]=1.[CH3:11][S:12](Cl)(=[O:14])=[O:13].O.C(OCC)(=O)C>N1C=CC=CC=1>[CH3:11][S:12]([O:1][C:2]1[CH:3]=[C:4]([B:8]([OH:10])[OH:9])[CH:5]=[CH:6][CH:7]=1)(=[O:14])=[O:13]

参加物

6

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 31297Methanesulfonyl chlorideHCID 2734359(3-hydroxyphenyl)boronic Acid

生成物 1

HCID 595685463-(Methylsulfonyloxy)phenylboronic acid

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To 3-hydroxyphenylboronic acid (10 g) stirred in pyridine (40 mL) at 0° C. was added methanesulfonyl chloride (8 mL). The reaction mixture was stirred for 1 h at room temperature and then water and ethyl acetate was added. The organic layer was separated and the aqueous layer was extracted with ethyl acetate. The combined organic layers were washed with dilute HCl washed with brine, dried over magnesium sulfate. The resulting solid was recrystallizated from petroleum ether and ethyl acetate to give the sub-titled compound (12 g).

後処理

  1. customThe organic layer was separated
  2. extractionthe aqueous layer was extracted with ethyl acetate
  3. washThe combined organic layers were washed with dilute HCl
  4. washwashed with brine
  5. dry with materialdried over magnesium sulfate

出典と根拠

ORDレコード
ord-aad4af688c5041da92cf3c20de86cadc
出典データセット
uspto-grants-2012_06
特許番号
US08193239B2

関連ノート

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