Hydrochloric Acid → HCID 21091024, 화합물

HRID 351262노트

반응식

HRID 351262 반응식
[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

참가 물질

6

반응물 2

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

생성물 1

HCID 21091024HCID 21091024, 화합물

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-27c98776ff2a4a328888a6a7498e7eec
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07183306B2

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