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

HRID 245508노트

반응식

HRID 245508 반응식
[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]

참가 물질

5

반응물 1

HCID 67356869(6,7-Difluoro-3-methyl-1,2-benzisoxazol-5-yl)methanol2회

생성물 1

HCID 86658113HCID 86658113, 화합물수율 92.5%

시약·촉매·용매 3

HCID 14801Manganese dioxide촉매HCID 178418406HCID 178418406, 화합물촉매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e75557fc1e6645f4924489f11d8a7053
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08658641B2

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