Pyridine → N3-(2,6-Dioxomorpholinoethyl)-N6-(ethoxycarbonylmethyl)-3,6-diazaoctanedioic Acid

HRID 1791087ノート

反応式

HRID 1791087 の反応式
[C:1]([CH2:4][N:5]([CH2:10][CH2:11][N:12]([CH2:26][C:27]([OH:29])=[O:28])[CH2:13][CH2:14][N:15]([CH2:20][C:21]([O:23][CH2:24][CH3:25])=[O:22])[CH2:16][C:17]([OH:19])=[O:18])[CH2:6][C:7]([OH:9])=O)([OH:3])=[O:2].N1C=CC=CC=1>C(OC(=O)C)(=O)C>[O:9]=[C:7]1[CH2:6][N:5]([CH2:10][CH2:11][N:12]([CH2:13][CH2:14][N:15]([CH2:20][C:21]([O:23][CH2:24][CH3:25])=[O:22])[CH2:16][C:17]([OH:19])=[O:18])[CH2:26][C:27]([OH:29])=[O:28])[CH2:4][C:1](=[O:2])[O:3]1

参加物

4

反応物 2

HCID 1049PyridineHCID 54279081Aadobenate Dimeglumine Impurity 3

生成物 1

HCID 15745373N3-(2,6-Dioxomorpholinoethyl)-N6-(ethoxycarbonylmethyl)-3,6-diazaoctanedioic Acid

試薬・触媒・溶媒 1

HCID 7918Acetic Anhydride溶媒

実験手順

A suspension of 21.1 g (50 mmol) of N3,N6-bis-(carboxymethyl)-N9-(ethoxy-carbonylmethyl)-3,6,9-triazaundecanedioic acid in 250 ml of acetic anhydride is allowed to stir for three days at room temperature after the addition of 42.2 ml of pyridine. Then, the precipitate is suctioned off, washed three times with 50 ml of acetic anhydride each and then stirred for several hours with absolute diethyl ether. After suctioning off, washing with absolute diethyl ether and drying in a vacuum at 40° C., 18.0 g (=89% of theory) of a white powder with a melting point of 195–196° C. is obtained.

後処理

  1. washwashed three times with 50 ml of acetic anhydride each and
  2. stirringthen stirred for several hours with absolute diethyl ether
  3. washwashing with absolute diethyl ether
  4. customdrying in a vacuum at 40° C.
  5. custom18.0 g (=89% of theory) of a white powder with a melting point of 195–196° C. is obtained

出典と根拠

ORDレコード
ord-02215aa8ae9d45eb9264057804da3dfe
出典データセット
uspto-grants-2006_07
特許番号
US07074387B2

反応ノート

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