(6,7-Difluoro-3-methyl-1,2-benzisoxazol-5-yl)methanol → HCID 86658113、化合物

HRID 577968ノート

反応式

HRID 577968 の反応式
[F:1][C:2]1[C:11]([CH2:12][OH:13])=[CH:10][C:5]2[C:6]([CH3:9])=[N:7][O:8][C:4]=2[C:3]=1[F:14]>C(Cl)Cl.[O-2].[O-2].[Mn+4].O=[Mn]=O>[F:1][C:2]1[C:11]([CH:12]=[O:13])=[CH:10][C:5]2[C:6]([CH3:9])=[N:7][O:8][C:4]=2[C:3]=1[F:14]

参加物

5

反応物 1

HCID 67356869(6,7-Difluoro-3-methyl-1,2-benzisoxazol-5-yl)methanol2 回

生成物 1

HCID 86658113HCID 86658113、化合物収率 92.5%

試薬・触媒・溶媒 3

HCID 14801Manganese dioxide触媒HCID 178418406HCID 178418406、化合物触媒HCID 6344Dichloromethane溶媒

実験手順

A mixture of (6,7-difluoro-3-methyl-1,2-benzisoxazol-5-yl)methanol (Intermediate 334, 0.7 g, 3.51 mmol) and manganese dioxide (6.11 g, 70.30 mmol) in CH2Cl2 (70 ml) was stirred at room temperature for 3 days. TLC shows conversion to a higher Rf spot with starting material. Additional MnO2 (5 g) was added and the mixture was heated to reflux for 24 hours. The mixture was filtered through celite and rinsed well with CH2Cl2. Solvent was removed from the filtrate to give 640 mg of product as a tan solid.

後処理

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 24 hours
  3. filtrationThe mixture was filtered through celite
  4. washrinsed well with CH2Cl2
  5. customSolvent was removed from the filtrate

出典と根拠

ORDレコード
ord-0745c48a18e8433fa518a26b6d0b307c
出典データセット
uspto-grants-2015_05
特許番号
US09040528B2

反応ノート

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