Sodium Bicarbonate → 5-(3-Acetoxy-2,2-diacetoxymethyl-propionylamino)-3-acetoxymethyl-N-(2,3-diacetoxypropyl)-2,4,6-triiodobenzamide

HRID 383038노트

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HRID 383038 반응식
[NH2:1][C:2]1[C:3]([I:29])=[C:4]([CH2:24][O:25][C:26](=[O:28])[CH3:27])[C:5]([I:23])=[C:6]([C:21]=1[I:22])[C:7]([NH:9][CH2:10][CH:11]([O:17][C:18](=[O:20])[CH3:19])[CH2:12][O:13][C:14](=[O:16])[CH3:15])=[O:8].[C:30]([O:33][CH2:34][C:35]([CH2:44][O:45][C:46](=[O:48])[CH3:47])([CH2:39][O:40][C:41](=[O:43])[CH3:42])[C:36](Cl)=[O:37])(=[O:32])[CH3:31].C(=O)([O-])O.[Na+]>CC(N(C)C)=O>[C:41]([O:40][CH2:39][C:35]([CH2:44][O:45][C:46](=[O:48])[CH3:47])([CH2:34][O:33][C:30](=[O:32])[CH3:31])[C:36]([NH:1][C:2]1[C:3]([I:29])=[C:4]([CH2:24][O:25][C:26](=[O:28])[CH3:27])[C:5]([I:23])=[C:6]([C:21]=1[I:22])[C:7]([NH:9][CH2:10][CH:11]([O:17][C:18](=[O:20])[CH3:19])[CH2:12][O:13][C:14](=[O:16])[CH3:15])=[O:8])=[O:37])(=[O:43])[CH3:42]

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 184291303-Acetoxymethyl-5-(2,3-diacetoxypropylaminocarbonyl)-2,4,6-triiodoanilineHCID 85706307HCID 85706307, 화합물

생성물 1

HCID 881689485-(3-Acetoxy-2,2-diacetoxymethyl-propionylamino)-3-acetoxymethyl-N-(2,3-diacetoxypropyl)-2,4,6-triiodobenzamide

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

반응 조건

온도
60 °C

실험 절차

5-Amino-3-acetoxymethyl-N-(2,3-diacetoxypropyl)-2,4,6-triiodobenzamide (1.05 g, 1.43 mmol) was dissolved in dimethylacetamide (2 ml) and added to trisacetoxymethylacetyl chloride (2.17 g, 7.4 mmol). The mixture was stirred at 60° C. for 5 days, and after cooling the mixture was added to an aqueous solution of sodium hydrogen carbonate (60 ml, 2%). The precipitate formed was filtered off and dissolved in chloroform (90 ml). The organic phase was washed with water (4×40 ml), dried (Na2SO4), and the solvent evaporated. A semisolid residue (1.16 g) was left, which according to MS analysis consisted of the two compounds: 5-(3-Acetoxy-2,2-diacetoxymethyl-propionylamino)-3-acetoxymethyl-N-(2,3-diacetoxypropyl)-2,4,6-triiodobenzamide with MS (ESP, m/e): 1002 ([M]+, 100%) and 5-acetamido-3-acetoxymethyl-N-(2,3-diacetoxypropyl)-2,4,6-triiodobenzamide with

후처리

  1. temperatureafter cooling the mixture
  2. customThe precipitate formed
  3. filtrationwas filtered off
  4. dissolutiondissolved in chloroform (90 ml)
  5. washThe organic phase was washed with water (4×40 ml)
  6. dry with materialdried (Na2SO4)
  7. customthe solvent evaporated
  8. waitA semisolid residue (1.16 g) was left

출처 및 근거

ORD 기록
ord-7df377fd6b1342a9adafba3c18a1ac45
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06310243B1

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