Glycolic Acid → HCID 20439386、化合物

HRID 1979536ノート

反応式

HRID 1979536 の反応式
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]

参加物

4

反応物 2

HCID 757Glycolic AcidHCID 178484962HCID 178484962、化合物

生成物 1

HCID 20439386HCID 20439386、化合物収率 0.7%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-925bfb0cf0f04e77b078278809814672
出典データセット
uspto-grants-1984_11
特許番号
US04481199

反応ノート

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