Glycolic Acid → HCID 178423363、化合物

HRID 1244317

反応式

HRID 1244317 の反応式
[NH2:1][C:2]1[C:7]([NH2:8])=[CH:6][CH:5]=[C:4]([CH3:9])[N:3]=1.[C:10](O)(=O)[CH2:11]O.S(Cl)([Cl:17])=O>C(Cl)(Cl)Cl>[ClH:17].[Cl:17][CH2:11][C:10]1[NH:1][C:2]2=[N:3][C:4]([CH3:9])=[CH:5][CH:6]=[C:7]2[N:8]=1

参加物

5

反応物 3

HCID 757Glycolic AcidHCID 24386Thionyl ChlorideHCID 27344206-Methylpyridine-2,3-diamine

生成物 1

HCID 178423363HCID 178423363、化合物収率 76.8%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

0.5 g 2,3-Diamino-6-methyl pyridine (4.0 mmol) and 0.37 g glycolic acid were heated at 150° C. for 1 h. The residue was suspended in chloroform (7.0 ml) treated with 1.5 ml thionyl chloride (20 mmol)for 4 h at reflux. The mixture was evaporated and the residue triturated with methanol. After concentration the residue was stirred over night in ether and the suspension was then filtered. The residue on the filter was dried to yield 0.67 g 2-chloromethyl-5-methyl-3H-imidazo[4,5-b]pyridine hydrochloride as a dark brown solid; M.p.: 225–230° C., (dec.).

後処理

  1. temperatureat reflux
  2. customThe mixture was evaporated
  3. customthe residue triturated with methanol
  4. concentrationAfter concentration the residue
  5. filtrationthe suspension was then filtered
  6. customThe residue on the filter was dried

出典と根拠

ORDレコード
ord-30fdcfd2e2b948c78acfda84ab1152c8
出典データセット
uspto-grants-2006_10
特許番号
US07122545B2

関連ノート

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