Acetic Acid → 6-Chloro-1H-imidazo[4,5-C]pyridine-4-carbonitrile

HRID 2079552ノート

反応式

HRID 2079552 の反応式
[NH2:1][C:2]1[C:3]([C:10]#[N:11])=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1[NH2:8].[CH2:12](OC(OCC)OCC)C.CC(O)=O>C(Cl)Cl>[Cl:9][C:5]1[N:4]=[C:3]([C:10]#[N:11])[C:2]2[N:1]=[CH:12][NH:8][C:7]=2[CH:6]=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 31214Ethyl orthoformateHCID 592183443,4-Diamino-6-chloropyridine-2-carbonitrile

生成物 1

HCID 451205836-Chloro-1H-imidazo[4,5-C]pyridine-4-carbonitrile

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 3,4-diamino-6-chloropicolinonitrile (3.2 g), triethylorthoformate (16 ml) and AcOH (5.4 ml) was heated to 150° C. in DCM (16 ml) in a microwave for 15 minutes. Solvent was evaporated, residue was dissolved in EtOAc (250 mL) and washed with water (150 mL). Organic layer was dried over sodium sulphate. Solvent was evaporated under reduced pressure to yield 6-chloro-1H-imidazo[4,5-c]pyridine-4-carbonitrile (2.2 g).

後処理

  1. customSolvent was evaporated
  2. dissolutionresidue was dissolved in EtOAc (250 mL)
  3. washwashed with water (150 mL)
  4. dry with materialOrganic layer was dried over sodium sulphate
  5. customSolvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-43b04cbf6f794fea943b7891296d06d4
出典データセット
uspto-grants-2011_04
特許番号
US07932251B2

反応ノート

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