Triacetoxyperiodinane → HCID 89522294、化合物

HRID 529714ノート

反応式

HRID 529714 の反応式
[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

参加物

4

反応物 2

HCID 159087TriacetoxyperiodinaneHCID 89522331HCID 89522331、化合物

生成物 1

HCID 89522294HCID 89522294、化合物収率 53%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-255c4a5f4b2e42e5be4cb08d4ae43876
出典データセット
uspto-grants-2016_05
特許番号
US09346825B2

反応ノート

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