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Glycolic Acid → HCID 10849575, 화합물

HRID 1601863
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HRID 1601863 반응식
[NH2:1][C:2]1[C:3]([NH:16][CH3:17])=[N:4][C:5]([O:8][CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[CH:6][CH:7]=1.[C:18]([OH:22])(=O)[CH2:19]O>>[CH2:9]([O:8][C:5]1[N:4]=[C:3]2[N:16]([CH3:17])[C:19]([CH2:18][OH:22])=[N:1][C:2]2=[CH:7][CH:6]=1)[C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 757Glycolic AcidHCID 107281183-Amino-6-benzyloxy-2-methylaminopyridine

생성물 1

HCID 10849575HCID 10849575, 화합물수율 46.5%

실험 절차

A procedure similar to that described in Preparation 43 was repeated, except that 7.50 g of 3-amino-6-benzyloxy-2-methylaminopyridine (prepared as described in Preparation 93) and 7.46 g of glycolic acid were reacted. After working up the product as described in Preparation 43, the resulting crude product was purifying by column chromatography through silica gel, using a 10:1 by volume mixture of ethyl acetate and methanol as the eluent, and was then crystallized by trituration with ethyl acetate, to give 4.10 g of the title compound, melting at 133-135° C.

후처리

  1. customA procedure similar to that described in Preparation 43
  2. customwere reacted
  3. customas described in Preparation 43
custom
the resulting crude product was purifying by column chromatography through silica gel
  • additionby volume mixture of ethyl acetate and methanol as the eluent
  • customwas then crystallized by trituration with ethyl acetate
  • 출처 및 근거

    ORD 기록
    ord-62743e3765a04615b2050e03c8f73ef2
    출처 데이터셋
    uspto-grants-1999_11
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US05977365

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