Triacetoxyperiodinane → HCID 89522294, 화합물

HRID 529714노트

반응식

HRID 529714 반응식
[Br:1][C:2]1[C:3]([CH2:11][OH:12])=[N:4][C:5]([N:8]([CH3:10])[CH3:9])=[N:6][CH:7]=1.CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O>C(Cl)Cl>[Br:1][C:2]1[C:3]([CH:11]=[O:12])=[N:4][C:5]([N:8]([CH3:9])[CH3:10])=[N:6][CH:7]=1

참가 물질

4

반응물 2

HCID 159087TriacetoxyperiodinaneHCID 89522331HCID 89522331, 화합물

생성물 1

HCID 89522294HCID 89522294, 화합물수율 53%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To [5-bromo-2-(dimethylamino)pyrimidin-4-yl]methanol (19 g, 82 mmol) in DCM (10 mL) was added Dess-Martin periodinane (41.7 g, 98 mmol) at room temperature. The reaction was stirred overnight and the reaction was diluted with hexanes, filtered and was concentrated before purification by column chromatography to yield 5-bromo-2-(dimethylamino)pyrimidine-4-carbaldehyde (10 g, 43.5 mmol). 1H NMR (500 MHz, CDCl3) δ 9.95 (s, 1H), 8.52 (s, 1H), 3.24 (s, 6H).

후처리

  1. filtrationfiltered
  2. concentrationwas concentrated before purification by column chromatography

출처 및 근거

ORD 기록
ord-255c4a5f4b2e42e5be4cb08d4ae43876
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09346825B2

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