Glycolic Acid → HCID 20439386, 화합물

HRID 1979536노트

반응식

HRID 1979536 반응식
I.[NH2:2][NH:3][C:4]([NH:23][CH3:24])=[N:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([CH2:16][N:17]2[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]2)[CH:11]=1.[C:25](O)(=O)[CH2:26][OH:27]>C1C=CC=CC=1>[CH3:24][N:23]1[C:4]([NH:5][CH2:6][CH2:7][CH2:8][O:9][C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([CH2:16][N:17]3[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22]3)[CH:11]=2)=[N:3][N:2]=[C:25]1[CH2:26][OH:27]

참가 물질

4

반응물 2

HCID 757Glycolic AcidHCID 178484962HCID 178484962, 화합물

생성물 1

HCID 20439386HCID 20439386, 화합물수율 0.7%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

N-Amino-N'-methyl-N"-[3-[3-(1-piperidinylmethyl)phenoxy]propyl]guanidine hydroiodide (2.24 g) and glycolic acid (1.52 g) were heated together for 3 h in dry benzene (25 ml) at reflux. The benzene was decanted from the residual oil, which was partitioned between ethyl acetate and aqueous 1N sodium hydroxide solution. The organic phase was chromatographed on silica using methanol to give a white solid. This solid was washed with boiling ethyl acetate to leave the title compound as a white solid (0.013 g) m.p. 151°-2°.

후처리

  1. temperatureat reflux
  2. customThe benzene was decanted from the residual oil, which
  3. customwas partitioned between ethyl acetate and aqueous 1N sodium hydroxide solution
  4. customThe organic phase was chromatographed on silica
  5. customto give a white solid
  6. washThis solid was washed with boiling ethyl acetate

출처 및 근거

ORD 기록
ord-925bfb0cf0f04e77b078278809814672
출처 데이터셋
uspto-grants-1984_11
특허 번호
US04481199

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