6-fluoro-3-[4-(phenylmethyl)piperazinyl]-1H-indazole → 6-fluoro-3-piperazin-1-yl-1H-indazole

HRID 2051013ノート

反応式

HRID 2051013 の反応式
[F:1][C:2]1[CH:10]=[C:9]2[C:5]([C:6]([N:11]3[CH2:16][CH2:15][N:14](CC4C=CC=CC=4)[CH2:13][CH2:12]3)=[N:7][NH:8]2)=[CH:4][CH:3]=1.[H][H]>[Ni].[Pd].CO>[F:1][C:2]1[CH:10]=[C:9]2[C:5]([C:6]([N:11]3[CH2:12][CH2:13][NH:14][CH2:15][CH2:16]3)=[N:7][NH:8]2)=[CH:4][CH:3]=1

参加物

6

反応物 2

HCID 150574536-fluoro-3-[4-(phenylmethyl)piperazinyl]-1H-indazoleHCID 178418361HCID 178418361、化合物

生成物 1

HCID 98158716-fluoro-3-piperazin-1-yl-1H-indazole収率 92%

試薬・触媒・溶媒 3

HCID 935Nickel触媒HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

A mixture of 12 parts of 6-fluoro-3-[4-(phenylmethyl)-piperazinyl]-1H-indazole, 1 part of Raney nickel catalyst and 200 parts of methanol was hydrogenated in a Parr-apparatus at normal pressure and at 50° C. with 2 parts of palladium-on-charcoal catalyst 10%. After the calculated amount of hydrogen was taken up, the catalyst was filtered off over diatomaceous earth and the filtrate was evaporated in vacuo. The residue was crystallized from acetonitrile. The product was filtered off and dried, yielding 7.7 parts (92.0%) of 6-fluoro-3-(1-piperazinyl)-1H-indazole (int. 8).

後処理

  1. filtrationthe catalyst was filtered off over diatomaceous earth
  2. customthe filtrate was evaporated in vacuo
  3. customThe residue was crystallized from acetonitrile
  4. filtrationThe product was filtered off
  5. customdried

出典と根拠

ORDレコード
ord-e917cc2fee1b4d01aa6d2c9be5496036
出典データセット
uspto-grants-1991_05
特許番号
US05015740

反応ノート

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