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Benzaldehyde → N-benzal-6-(methylthio)pyridine-3-amine

HRID 1523273
ノート
印刷プレビュー

反応式

HRID 1523273 の反応式
[CH3:1][S:2][C:3]1[CH:8]=[CH:7][C:6]([NH2:9])=[CH:5][N:4]=1.[CH:10](=O)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C(=O)([O-])[O-].[Na+].[Na+]>CC([O-])C.CC([O-])C.CC([O-])C.CC([O-])C.[Ti+4].O1CCCC1>[CH:10](=[N:9][C:6]1[CH:5]=[N:4][C:3]([S:2][CH3:1])=[CH:8][CH:7]=1)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=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 240BenzaldehydeHCID 10340Sodium CarbonateHCID 102611796-(Methylsulfanyl)pyridin-3-amine

生成物 1

HCID 89962644N-benzal-6-(methylthio)pyridine-3-amine

試薬・触媒・溶媒 2

HCID 11026Titanium isopropoxide触媒HCID 8028Tetrahydrofuran溶媒

実験手順

2-(methylthio)-5-aminopyridine (1 g, 7 mmol), benzaldehyde (0.76 g, 7 mmol), tetraisopropyl titanate (3 mL) and tetrahydrofuran (25 mL) were mixed and stirred to react at 70° C. for 24 hours. Saturated sodium carbonate solution was added into the reaction mixture, and the mixture was extracted with ethyl acetate for three times. The combined organic phase was dried with anhydrous sodium sulfate, filtered and concentrated to yield the residual (1.72 g), which was directly used in the next reaction step without purification.

後処理

  1. customto react at 70° C. for 24 hours
  2. extractionthe mixture was extracted with ethyl acetate for three times
  3. dry with materialThe combined organic phase was dried with anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customto yield the residual (1.72 g), which
  7. customwas directly used in the next reaction step without purification

出典と根拠

ORDレコード
ord-8de93fd91f2344f3bfd0aaed68e6a7ec
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09079876B2

反応ノート

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