Phosgene → HCID 18429324, 화합물

HRID 1280134

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HRID 1280134 반응식
[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]

참가 물질

7

반응물 3

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

생성물 1

HCID 18429324HCID 18429324, 화합물

시약·촉매·용매 3

HCID 16685285Hg(TFA)2촉매HCID 1140Toluene용매HCID 312751,4-Dioxane용매

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온도
60 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-c521745d17b4445a83de0f5063969d20
출처 데이터셋
uspto-grants-2002_09
특허 번호
US06448442B1

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