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Water → HCID 23158275、化合物

HRID 601678
ノート
印刷プレビュー

反応式

HRID 601678 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([CH:8]=[C:9]([C:11]([OH:13])=O)[N:10]=2)[CH:7]=1.Cl.[CH3:15][O:16][NH:17][CH3:18].Cl.CN(C)CCCN=C=NCC.O>N1C=CC=CC=1>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([CH:8]=[C:9]([C:11](=[O:13])[N:17]([O:16][CH3:15])[CH3:18])[N:10]=2)[CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27570186-Bromoimidazo(1,2-a)pyridine-2-carboxylic acid

生成物 1

HCID 23158275HCID 23158275、化合物収率 36.1%

試薬・触媒・溶媒 1

HCID 1049
Pyridine
溶媒

実験手順

850 mg of 6-bromo-2-hydroxycarbonyl-imidazo[1,2-a]pyridine, 519 mg of N-methoxy-N-methyl-amine hydrochloride, and 1.12 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride were dissolved in 10 ml of pyridine, and the mixture was stirred at room temperature for 2 days. Water was added to the obtained solution, and the products were extracted with ethyl acetate. Organic layer was washed with saturated sodium chloride aqueous solution, and dried with anhydrous magnesium sulfate. Then, the solvents were distilled outunder reduced pressure. The obtained residues were purified by silicagel column chromatography (ethyl acetate) to obtain 362 mg of the above compound.

後処理

  1. extractionthe products were extracted with ethyl acetate
  2. washOrganic layer was washed with saturated sodium chloride aqueous solution
  3. dry with materialdried with anhydrous magnesium sulfate
  4. distillationThen, the solvents were distilled outunder reduced pressure
  5. customThe obtained residues were purified by silicagel column chromatography (ethyl acetate)

出典と根拠

ORDレコード
ord-2fb6a568fa9449d09a2fc8f2d2fa2726
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07902369B2

反応ノート

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