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Sodium Iodide → Acetyloxvmethyl 5-(N-acetylamino)-3-(N-acetyl-N-methylamino)-2,4,6-triiodobenzenecarboxylate

HRID 1707551
ノート
印刷プレビュー

反応式

HRID 1707551 の反応式
Cl[CH2:2][O:3][C:4](=[O:6])[CH3:5].[C:7]([NH:10][C:11]1[C:12]([I:27])=[C:13]([N:22]([C:24](=[O:26])[CH3:25])[CH3:23])[C:14]([I:21])=[C:15]([C:18]([O-:20])=[O:19])[C:16]=1[I:17])(=[O:9])[CH3:8].[Cs+].[I-].[Na+]>CN(C=O)C>[C:7]([NH:10][C:11]1[C:12]([I:27])=[C:13]([N:22]([C:24](=[O:26])[CH3:25])[CH3:23])[C:14]([I:21])=[C:15]([C:18]([O:20][CH2:2][O:3][C:4](=[O:6])[CH3:5])=[O:19])[C:16]=1[I:17])(=[O:9])[CH3:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 5238Sodium IodideHCID 69366Chloromethyl acetateHCID 23675689cesium 5-(N-acetylamino)-3-(N-acetyl-N-methylamino)-2,4,6-triiodobenzenecarboxylate

生成物 1

HCID 17807105Acetyloxvmethyl 5-(N-acetylamino)-3-(N-acetyl-N-methylamino)-2,4,6-triiodobenzenecarboxylate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

Chloromethylacetate (Neuenschwander, Markus et. al., Helv. Chim. Acta, 61 (1978) 2047) (2.30 g, 21.2 mmol) in dry DMF (100 ml) is added dropwise at 50° C. to a solution of cesium 5-(N-acetylamino)-3-(N-acetyl-N-methylamino)-2,4,6-triiodobenzenecarboxylate (13.4 g, 17.7 mmol) and sodium iodide (133 mg, 0.89 mmol) in dry DMF (210 ml). The precipitate is removed by filtration after stirring for 21 hours and the solvent is removed at reduced pressure. The residue is dissolved in chloroform (200 ml) and washed four times with a saturated sodium hydrogen carbonate solution. After drying with magnesium sulfate the solvent is removed at reduced pressure to give the title compound:

後処理

  1. customThe precipitate is removed by filtration
  2. customthe solvent is removed at reduced pressure
  3. dissolutionThe residue is dissolved in chloroform (200 ml)
  4. washwashed four times with a saturated sodium hydrogen carbonate solution
  5. dry with materialAfter drying with magnesium sulfate the solvent
  6. customis removed at reduced pressure

出典と根拠

ORDレコード
ord-74a2d873e5874faf8c6840a825c9ea64
出典データセット
uspto-grants-1994_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05354549

反応ノート

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