Ammonia → HCID 178519929, 화합물

HRID 55491노트

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HRID 55491 반응식
[C:1]([OH:5])(=O)[CH2:2]O.[Cl:6][C:7]1[N:12]=[C:11]([NH2:13])[C:10]([NH2:14])=[CH:9][CH:8]=1.Cl.N>>[Cl:6][C:7]1[N:12]=[C:11]2[NH:13][C:2]([CH2:1][OH:5])=[N:14][C:10]2=[CH:9][CH:8]=1

참가 물질

5

반응물 4

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 757Glycolic AcidHCID 106306156-Chloropyridine-2,3-diamine

생성물 1

HCID 178519929HCID 178519929, 화합물수율 83.4%

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온도
150 °C

실험 절차

6.60 g of glycolic acid were added to 5.00 g of 6-chloro-2,3-diaminopyridine (prepared as described in Preparation 42), and the resulting mixture was stirred at 150° C. for 4 hours. At the end of this time, the reaction mixture was treated with 3N aqueous hydrochloric acid and subsequently made alkaline by the addition of aqueous ammonia. The aqueous mixture was evaporated to dryness, and the resulting residue was purified by column chromatography through silica gel, using a gradient elution method, with mixtures of ethyl acetate and methanol in ratios ranging from 1:0 to 10:1 by volume as the eluent. The product was then crystallized by trituration with ethyl acetate, to give 5.33 g of the title compound, melting at 224°-226° C.

후처리

  1. customThe aqueous mixture was evaporated to dryness
  2. customthe resulting residue was purified by column chromatography through silica gel
  3. washa gradient elution method
  4. customThe product was then crystallized by trituration with ethyl acetate

출처 및 근거

ORD 기록
ord-635b4ec7e35d4c8e9528b9b32b08a17f
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05624935

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