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Methanol → N-(4-{2-[4-(aminomethyl)-3-fluorophenyl]ethyl}-1,3-thiazol-2-yl)acetamide

HRID 1892522
ノート
印刷プレビュー

反応式

HRID 1892522 の反応式
[N:1]([CH2:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11][CH2:12][C:13]2[N:14]=[C:15]([NH:18][C:19](=[O:21])[CH3:20])[S:16][CH:17]=2)=[CH:7][C:6]=1[F:22])=[N+]=[N-].CO>C(OCC)(=O)C.[C].[Pd]>[NH2:1][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11][CH2:12][C:13]2[N:14]=[C:15]([NH:18][C:19](=[O:21])[CH3:20])[S:16][CH:17]=2)=[CH:7][C:6]=1[F:22]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 887MethanolHCID 86650022N-(4-{2-[4-(azidomethyl)-3-fluorophenyl]ethyl}-1,3-thiazol-2-yl)acetamide

生成物 1

HCID 86650023N-(4-{2-[4-(aminomethyl)-3-fluorophenyl]ethyl}-1,3-thiazol-2-yl)acetamide収率 85.3%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 8857Ethyl Acetate溶媒2 回

実験手順

To a solution of N-(4-{2-[4-(azidomethyl)-3-fluorophenyl]ethyl}-1,3-thiazol-2-yl)acetamide (152.3 mg, 0.477 mmol) in ethyl acetate (21 ml) was added 10% palladium carbon (30.5 mg, containing 50% water), and the mixture was hydrogenated at room temperature under an atmospheric pressure. Ethyl acetate (5 ml) and methanol (5 ml) were added to the reaction mixture, and the mixture was filtered through celite. The filtrate was concentrated under reduced pressure, and the resulting solid was collected by filtration, washed with tert-butyl methyl ether (5 ml) and dried under reduced pressure to give N-(4-{2-[4-(aminomethyl)-3-fluorophenyl]ethyl}-1,3-thiazol-2-yl)acetamide (119.3 mg, 0.407 mmol, yield 85.3%) as a white solid.

後処理

  1. customwas hydrogenated at room temperature under an atmospheric pressure
  2. filtrationthe mixture was filtered through celite
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. filtrationthe resulting solid was collected by filtration
  5. washwashed with tert-butyl methyl ether (5 ml)
  6. customdried under reduced pressure

出典と根拠

ORDレコード
ord-2c25d360d6124fd59c9e87daa2f1fa31
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08507690B2

反応ノート

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