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Hydrochloric Acid → 4-Aminomethyl-2-(4-fluorophenyl)-3-(pyridin-4-yl)-1H-pyrrole Dihydrochloride

HRID 1244985
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HRID 1244985 반응식
[ClH:1].CO[N:4]=[CH:5][C:6]1[C:10]([C:11]2[CH:16]=[CH:15][N:14]=[CH:13][CH:12]=2)=[C:9]([C:17]2[CH:22]=[CH:21][C:20]([F:23])=[CH:19][CH:18]=2)[NH:8][CH:7]=1.C(OCC)C>[Pd].CO>[ClH:1].[ClH:1].[NH2:4][CH2:5][C:6]1[C:10]([C:11]2[CH:12]=[CH:13][N:14]=[CH:15][CH:16]=2)=[C:9]([C:17]2[CH:18]=[CH:19][C:20]([F:23])=[CH:21][CH:22]=2)[NH:8][CH:7]=1
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참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 1363804435-(4-Fluorophenyl)-4-(pyridin-4-yl)-1H-pyrrole-3-carboxaldehyde O-methyloxime

생성물 1

HCID 219227564-Aminomethyl-2-(4-fluorophenyl)-3-(pyridin-4-yl)-1H-pyrrole Dihydrochloride수율 68%

시약·촉매·용매 2

HCID 23938Palladium촉매
HCID 887
Methanol
용매

실험 절차

10 ml of 10% hydrochloric acid and 0.50 g of 10% palladium on carbon were added to a solution of 497 mg (1.68 mmol) of 5-(4-fluorophenyl)-4-(pyridin-4-yl)-1H-pyrrole-3-carboxaldehyde O-methyloxime [which was prepared as described in step 5(i) above] in 10 ml of methanol. The mixture was stirred under a hydrogen atmosphere at room temperature for 2 hours. At the end of this time, the reaction mixture was filtered and the filtrate thus obtained was concentrated by evaporation under reduced pressure. The residue was washed with diisopropylether and then with diethylether to give 391 mg (yield 68%) of the title compound as a yellowish orange powder.

후처리

  1. filtrationAt the end of this time, the reaction mixture was filtered
  2. customthe filtrate thus obtained
  3. concentrationwas concentrated by evaporation under reduced pressure
  4. washThe residue was washed with diisopropylether

출처 및 근거

ORD 기록
ord-1d2786f03a764c9b814277402c53c70a
출처 데이터셋
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07122666B2

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