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

HRID 1523273
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HRID 1523273 반응식
[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
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참가 물질

6

반응물 3

HCID 240BenzaldehydeHCID 10340Sodium CarbonateHCID 102611796-(Methylsulfanyl)pyridin-3-amine

생성물 1

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

시약·촉매·용매 2

HCID 11026Titanium isopropoxide촉매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8de93fd91f2344f3bfd0aaed68e6a7ec
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09079876B2

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