HCID 14625291、化合物 → HCID 14517660、化合物

HRID 2352453ノート

反応式

HRID 2352453 の反応式
[Cl:1][C:2]1[N:3]([C:11]2[CH:16]=[C:15]([N+:17]([O-])=O)[C:14]([O:20][CH2:21][C:22](OCCCC)=[O:23])=[CH:13][C:12]=2[F:29])[N:4]=[C:5]2[C:10]=1[CH2:9][CH2:8][CH2:7][CH2:6]2>C(O)(=O)C.[Fe]>[Cl:1][C:2]1[N:3]([C:11]2[C:12]([F:29])=[CH:13][C:14]3[O:20][CH2:21][C:22](=[O:23])[NH:17][C:15]=3[CH:16]=2)[N:4]=[C:5]2[C:10]=1[CH2:9][CH2:8][CH2:7][CH2:6]2

参加物

4

反応物 1

HCID 14625291HCID 14625291、化合物

生成物 1

HCID 14517660HCID 14517660、化合物収率 82.1%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 176Acetic Acid溶媒

実験手順

A suspension of 3-chloro-2-(2-fluoro-4-butyloxycarbonylmethoxy-5-nitrophenyl)-4,5,6,7-tetrahydro-2H-indazole (10 g) and iron powders (10 g) in acetic acid was refluxed for 5 hours. After completion of the reaction, the reaction mixture was filtered by the use of celite, and the filtrate was combined with water and extracted with ethyl acetate. The oragnic layer was concentrated, and the residue was purified by column chromatography using a mixture of hexane and ethyl acetate as an eluent to give 3-chloro-2-[7-fluoro-2H-1,4-benzoxazine-3(4H)-on-6-yl]-4,5,6,7-tetrahydro-2H-indazole (6.2 g). nD29.0 1.5628.

後処理

  1. temperaturewas refluxed for 5 hours
  2. customAfter completion of the reaction
  3. filtrationthe reaction mixture was filtered by the use of celite
  4. extractionextracted with ethyl acetate
  5. concentrationThe oragnic layer was concentrated
  6. customthe residue was purified by column chromatography
  7. additiona mixture of hexane and ethyl acetate as an eluent

出典と根拠

ORDレコード
ord-631a9f9bbfd746e4bb1f8c84f9e16a41
出典データセット
uspto-grants-1989_10
特許番号
US04877444

反応ノート

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