2-(4-Chloro-2-(tetrahydropyran-4-yl)aminonitrobenzen-5-yl)benzoxazole → HCID 67498666、化合物

HRID 74295ノート

反応式

HRID 74295 の反応式
[Cl:1][C:2]1[C:7]([C:8]2[O:9][C:10]3[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=3[N:12]=2)=[CH:6][C:5]([N+:17]([O-])=O)=[C:4]([NH:20][CH:21]2[CH2:26][CH2:25][O:24][CH2:23][CH2:22]2)[CH:3]=1>[Fe].C(O)(=O)C>[Cl:1][C:2]1[C:7]([C:8]2[O:9][C:10]3[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=3[N:12]=2)=[CH:6][C:5]([NH2:17])=[C:4]([NH:20][CH:21]2[CH2:26][CH2:25][O:24][CH2:23][CH2:22]2)[CH:3]=1

参加物

4

反応物 1

HCID 674991902-(4-Chloro-2-(tetrahydropyran-4-yl)aminonitrobenzen-5-yl)benzoxazole

生成物 1

HCID 67498666HCID 67498666、化合物収率 65%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 176Acetic Acid溶媒

実験手順

To 2-(4-chloro-2-(tetrahydropyran-4-yl)aminonitrobenzen-5-yl)benzoxazole (see Working Example 112-2) (0.10 g, 0.8 mmol) was added iron powder (0.33 g, 5.8 mmol) and acetic acid (50 mL), and this was heated to reflux for 2 hours. After the reaction solution cooled, this was filtered through Celite and concentrated, and the residue obtained was purified by silica gel column chromatography to yield the title compound (0.06 g, 65% yield) as a reddish-brown solid.

後処理

  1. temperaturethis was heated
  2. temperatureto reflux for 2 hours
  3. temperatureAfter the reaction solution cooled
  4. filtrationthis was filtered through Celite
  5. concentrationconcentrated
  6. customthe residue obtained
  7. customwas purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-51ba33be36ca41aba9b8486e6733c2a6
出典データセット
uspto-grants-2014_09
特許番号
US08829035B2

反応ノート

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