Glycolic Acid → HCID 178423363, 화합물

HRID 1244317

반응식

HRID 1244317 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 178423363HCID 178423363, 화합물수율 76.8%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-30fdcfd2e2b948c78acfda84ab1152c8
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07122545B2

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