Hydrochloric Acid → HCID 21091024、化合物

HRID 351262ノート

反応式

HRID 351262 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]2[N:13]([C:14]3[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=3)[N:12]=[C:11]([C:22]([O:24][CH2:25][CH3:26])=[O:23])[CH:10]=2)=[CH:5][CH:4]=1)#[N:2].[ClH:27]>C1COCC1.CO.[Pd]>[ClH:27].[NH2:2][CH2:1][C:3]1[CH:4]=[CH:5][C:6]([C:9]2[N:13]([C:14]3[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=3)[N:12]=[C:11]([C:22]([O:24][CH2:25][CH3:26])=[O:23])[CH:10]=2)=[CH:7][CH:8]=1

参加物

6

反応物 2

HCID 313Hydrochloric AcidHCID 21091028ethyl 5-(4-cyanophenyl)-1-(4-methoxyphenyl)-1H-pyrazole-3-carboxylate

生成物 1

HCID 21091024HCID 21091024、化合物

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 10% Pd-C 50% wet (100 mg) and ethyl 5-(4-cyanophenyl)-1-(4-methoxyphenyl)-1H-pyrazole-3-carboxylate (1 g) in THF (10 ml), MeOH (5 ml), and 1M HCl (2.9 ml) was hydrogenated under H2 latmat ambient temperature for 6.5 hours. The catalyst was filtered off through a celite pad and the pad was washed with MeOH. The filtrate and combined washings were concentrated in vacuo. The residue was dissolved in EtOH and concentrated in vacuo. The residue was crystallized from AcOEt to give ethyl 5-[4-(aminomethyl)phenyl]-1-(4-methoxyphenyl)-1H-pyrazole-3-carboxylate hydrochloride (984 mg) as a powder.

後処理

  1. filtrationThe catalyst was filtered off through a celite pad
  2. washthe pad was washed with MeOH
  3. concentrationwere concentrated in vacuo
  4. dissolutionThe residue was dissolved in EtOH
  5. concentrationconcentrated in vacuo
  6. customThe residue was crystallized from AcOEt

出典と根拠

ORDレコード
ord-27c98776ff2a4a328888a6a7498e7eec
出典データセット
uspto-grants-2007_02
特許番号
US07183306B2

反応ノート

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