3-Hydroxymethyl-5-dichloromethyl-2-phthalimidopyrazine → 3-Formyl-5-dichloromethyl-2-phthalimidopyrazine

HRID 4441

反応式

HRID 4441 の反応式
[Cr](Cl)([O-])(=O)=O.[NH+]1C=CC=CC=1.[OH:12][CH2:13][C:14]1[C:15]([N:23]2[C:27](=[O:28])[C:26]3=[CH:29][CH:30]=[CH:31][CH:32]=[C:25]3[C:24]2=[O:33])=[N:16][CH:17]=[C:18]([CH:20]([Cl:22])[Cl:21])[N:19]=1>ClCCl>[CH:13]([C:14]1[C:15]([N:23]2[C:24](=[O:33])[C:25]3=[CH:32][CH:31]=[CH:30][CH:29]=[C:26]3[C:27]2=[O:28])=[N:16][CH:17]=[C:18]([CH:20]([Cl:21])[Cl:22])[N:19]=1)=[O:12]

参加物

4

反応物 2

HCID 136047773-Hydroxymethyl-5-dichloromethyl-2-phthalimidopyrazineHCID 178418287HCID 178418287、化合物

生成物 1

HCID 136047783-Formyl-5-dichloromethyl-2-phthalimidopyrazine収率 78%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

5.1 g of pyridinium chlorochromate were added a little at a time to a solution of 4 g of 3-hydroxymethyl-5-dichloromethyl-2-phthalimidopyrazine in 80 ml of dichloromethane at 35° C., after which the mixture was stirred for 40 minutes and filtered over silica gel, and the filtrate was evaporated down. 3.1 g (76%) of colorless crystals of 3-formyl-5-dichloromethyl-2-phthalimidopyrazine of melting point 145°-146° C. (from ethyl acetate) were obtained. 1H-NMR (270 MHz, CDCl3): δ6.9 (s, 1H), 8.0 (m, 4H), 9.3 (s, 1H), 10.1 (s, 1H).

後処理

  1. filtrationfiltered over silica gel
  2. customthe filtrate was evaporated down

出典と根拠

ORDレコード
ord-0e6c16dd3649420f8ec300810a013520
出典データセット
uspto-grants-1988_02
特許番号
US04725689

関連ノート

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