Acetic Anhydride → 3-Acetoxymethyl-5-(2,3-diacetoxypropylaminocarbonyl)-2,4,6-triiodoaniline

HRID 618940노트

반응식

HRID 618940 반응식
[OH:1][CH2:2][C:3]1[C:4]([I:20])=[C:5]([C:7]([I:19])=[C:8]([C:11]([NH:13][CH2:14][CH:15]([OH:18])[CH2:16][OH:17])=[O:12])[C:9]=1[I:10])[NH2:6].C(O[C:25](=[O:27])[CH3:26])(=O)C>N1C=CC=CC=1>[C:2]([O:1][CH2:2][C:3]1[C:4]([I:20])=[C:5]([C:7]([I:19])=[C:8]([C:11]([NH:13][CH2:14][CH:15]([O:18][C:25](=[O:27])[CH3:26])[CH2:16][O:17][C:11](=[O:12])[CH3:8])=[O:12])[C:9]=1[I:10])[NH2:6])(=[O:1])[CH3:3]

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 184291813-Hydroxymethyl-5-(2,3-dihydroxypropylaminocarbonyl)-2,4,6-triiodoaniline

생성물 1

HCID 184291303-Acetoxymethyl-5-(2,3-diacetoxypropylaminocarbonyl)-2,4,6-triiodoaniline

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

3-Hydroxymethyl-5-(2,3-dihydroxypropylaminocarbonyl)-2,4,6-triiodoaniline (1.32 g, 2.1 mmol) was dissolved in pyridine (10 ml) containing acetic anhydride (10 ml). The mixture was stirred at room temperature for 2 h and CH2Cl2 (100 ml) and the solution was washed with water (3×25 ml). The organic phase was washed with water (3×50 ml) and a saturated aqueous solution of NaHCO3 (2×50 ml). After drying (Na2SO4) and evaporation, the residue was purified by flash chromatography on a silica column using a mixture of CH2Cl2 and methanol (95:5) as the eluent. Yield: 1.30 g (82%).

후처리

  1. washCH2Cl2 (100 ml) and the solution was washed with water (3×25 ml)
  2. washThe organic phase was washed with water (3×50 ml)
  3. customAfter drying
  4. custom(Na2SO4) and evaporation
  5. customthe residue was purified by flash chromatography on a silica column
  6. additiona mixture of CH2Cl2 and methanol (95:5) as the eluent

출처 및 근거

ORD 기록
ord-750415f901ae430d8bc53cdcbf1848e2
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05958375

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