HCID 86722244、化合物 → HCID 178488264、化合物

HRID 869400ノート

反応式

HRID 869400 の反応式
[Cl:1][C:2]1[C:7]2[C:8]3[NH:9][CH:10]([C:16]4[N:17]=[C:18]([NH:21][C:22](=[O:26])[CH:23]([CH3:25])[CH3:24])[S:19][CH:20]=4)[CH2:11][C:12](=[O:15])[C:13]=3[O:14][C:6]=2[CH:5]=[CH:4][C:3]=1[O:27][CH3:28]>C1COCC1.O=[Mn]=O>[OH:15][C:12]1[CH:11]=[C:10]([C:16]2[N:17]=[C:18]([NH:21][C:22](=[O:26])[CH:23]([CH3:25])[CH3:24])[S:19][CH:20]=2)[N:9]=[C:8]2[C:7]3[C:2]([Cl:1])=[C:3]([O:27][CH3:28])[CH:4]=[CH:5][C:6]=3[O:14][C:13]=12

参加物

4

反応物 1

HCID 86722244HCID 86722244、化合物

生成物 1

HCID 178488264HCID 178488264、化合物収率 60.3%

試薬・触媒・溶媒 2

HCID 14801Manganese dioxide触媒HCID 8028Tetrahydrofuran溶媒

実験手順

11F (500 mg, 1.19 mmol) was dissolved in THF (tetrahydrofuran, 30 mL). To the solution was added activated MnO2 (600 mg, 6 eq, 6.9 mmol). The mixture was refluxed for 48 hours. After reaction completed, the mixture was cooled and filtered. The cake was washed well with THF and MeOH. The filtrate was concentrated and purified by column chromatography on silica gel to give 300 mg of pure product (11G).

後処理

  1. temperatureThe mixture was refluxed for 48 hours
  2. customAfter reaction
  3. temperaturethe mixture was cooled
  4. filtrationfiltered
  5. washThe cake was washed well with THF and MeOH
  6. concentrationThe filtrate was concentrated
  7. custompurified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-04f9cea192bf4e1eb39e89784a8d9ef5
出典データセット
uspto-grants-2015_03
特許番号
US08969373B2

反応ノート

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