Potassium Carbonate → 6-[(3-Chloro-pyridin-4-ylmethyl)-amino]-pyridine-3-carbaldehyde

HRID 1754742노트

반응식

HRID 1754742 반응식
[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[CH2:8][NH:9][C:10]1[N:15]=[CH:14][C:13]([CH2:16][OH:17])=[CH:12][CH:11]=1.CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O.C(=O)([O-])[O-].[K+].[K+]>O1CCCC1>[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[CH2:8][NH:9][C:10]1[N:15]=[CH:14][C:13]([CH:16]=[O:17])=[CH:12][CH:11]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 159087TriacetoxyperiodinaneHCID 576192366-[(3-Chloro-pyridin-4-ylmethyl)-amino]pyridin-3-yl-methanol

생성물 1

HCID 576192126-[(3-Chloro-pyridin-4-ylmethyl)-amino]-pyridine-3-carbaldehyde수율 91%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To 6-[(3-chloro-pyridin-4-ylmethyl)-amino]-pyridin-3-yl-methanol (556, 0.50 g, 2.00 mmol) in tetrahydrofuran (20.0 mL) was added Dess-Martin periodinane (1.02 g, 2.40 mmol). The reaction was stirred at room temperature for 10 minutes, then poured into aqueous potassium carbonate, and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated to give crude compound (557, 0.45 g, 91%) that was used in the next step without further purification.

후처리

  1. extractionextracted with ethyl acetate
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated

출처 및 근거

ORD 기록
ord-26dd6933a6f942c29d4f311eb5e26ece
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09169250B2

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