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

HRID 1244985
ノート
印刷プレビュー

反応式

HRID 1244985 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒
HCID 887
Methanol
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1d2786f03a764c9b814277402c53c70a
出典データセット
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07122666B2

反応ノート

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