Phosgene → HCID 18429324、化合物

HRID 1280134

反応式

HRID 1280134 の反応式
[C:1]([O:4][CH:5]([CH2:34][O:35][C:36](=[O:38])[CH3:37])[CH2:6][NH:7][C:8]([C:10]1[C:11]([I:33])=[C:12]([C:14]([I:32])=[C:15]([C:18]([NH:20][CH2:21][CH:22]([O:28][C:29](=[O:31])[CH3:30])[CH2:23][O:24][C:25](=[O:27])[CH3:26])=[O:19])[C:16]=1[I:17])[NH2:13])=[O:9])(=[O:3])[CH3:2].[C:39](Cl)(Cl)=[O:40].[C:43]([O:46][CH2:47][C:48]1[C:49]([I:71])=[C:50]([C:52]([I:70])=[C:53]([C:56]([NH:58][CH2:59][CH:60]([O:66][C:67](=[O:69])[CH3:68])[CH2:61][O:62][C:63](=[O:65])[CH3:64])=[O:57])[C:54]=1[I:55])[NH2:51])(=[O:45])[CH3:44]>O1CCOCC1.C1(C)C=CC=CC=1.[Hg](OC(C(F)(F)F)=O)OC(C(F)(F)F)=O>[C:43]([O:46][CH2:47][C:48]1[C:49]([I:71])=[C:50]([NH:51][C:39]([NH:13][C:12]2[C:11]([I:33])=[C:10]([C:8]([NH:7][CH2:6][CH:5]([O:4][C:1](=[O:3])[CH3:2])[CH2:34][O:35][C:36](=[O:38])[CH3:37])=[O:9])[C:16]([I:17])=[C:15]([C:18]([NH:20][CH2:21][CH:22]([O:28][C:29](=[O:31])[CH3:30])[CH2:23][O:24][C:25](=[O:27])[CH3:26])=[O:19])[C:14]=2[I:32])=[O:40])[C:52]([I:70])=[C:53]([C:56]([NH:58][CH2:59][CH:60]([O:66][C:67](=[O:69])[CH3:68])[CH2:61][O:62][C:63](=[O:65])[CH3:64])=[O:57])[C:54]=1[I:55])(=[O:45])[CH3:44]

参加物

7

反応物 3

HCID 6371PhosgeneHCID 98975345-Amino-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-benzenedicarboxamide TetraacetateHCID 18429130HCID 18429130、化合物

生成物 1

HCID 18429324HCID 18429324、化合物

試薬・触媒・溶媒 3

HCID 16685285Hg(TFA)2触媒HCID 1140Toluene溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
60 °C

実験手順

3,5-Bis(2,3-diacetoxypropylaminocarbonyl)-2,4,6-triiodoaniline (260 mg, 0.30 mmol) was dissolved in dioxane (1.0 ml) and a solution of phosgene in toluene (1.93 M, 1.8 ml) was added. The flask was tightly sealed and then heated to 60° C. for 17 h. After cooling to room temperature, the solvent was distilled off at reduced pressure. Dioxane (3 ml) was added and distilled off again. This procedure was repeated twice. Dioxane (1 ml) was added followed by 3-acetoxymethyl-5-(2,3-diacetoxypropylaminocarbonyl)-2,4,6-triiodoaniline (0.245 g, 0.31 mmol), prepared according to Example 16a, and Hg(OCOCF3)2 (20 mg). The mixture was stirred for 16 h at room temperature, the solvent was evaporated and the residue was purified by preparative HPLC. Yield: 0.192 g (39%).

後処理

  1. customThe flask was tightly sealed
  2. temperatureAfter cooling to room temperature
  3. distillationthe solvent was distilled off at reduced pressure
  4. additionDioxane (3 ml) was added
  5. distillationdistilled off again
  6. additionDioxane (1 ml) was added
  7. customprepared
  8. customthe solvent was evaporated
  9. customthe residue was purified by preparative HPLC

出典と根拠

ORDレコード
ord-c521745d17b4445a83de0f5063969d20
出典データセット
uspto-grants-2002_09
特許番号
US06448442B1

関連ノート

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