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

HRID 1595118노트

반응식

HRID 1595118 반응식
[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

참가 물질

4

반응물 2

HCID 1049PyridineHCID 54279081Aadobenate Dimeglumine Impurity 3

생성물 1

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

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bb880d48ddcc447bb61d3a58a94fc259
출처 데이터셋
uspto-grants-2001_09
특허 번호
US06287538B1

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