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

HRID 1418274노트

반응식

HRID 1418274 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(Cl)Cl>C(OC(=O)C)(=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:16](=[O:17])[CH3:15])[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

5

반응물 2

HCID 6344DichloromethaneHCID 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 2

HCID 1049Pyridine용매HCID 7918Acetic Anhydride용매

실험 절차

3-Hydroxymethyl-5-(2,3-dihydroxypropylaminocarbonyl)-2,4,6-triiodoaniline (1.89 g, 3.06 mmol) prepared according to Example 3d, was dissolved in a mixture of acetic anhydride (5 ml) and pyridine (5 ml). The mixture was stirred at room temperature for 24 h, CH2Cl2 (100 ml) was added and the solution was washed with water (3×25 ml), with a saturated aqueous solution of NaHCO3, dried (Na2SO4) and evaporated. The product was purified by flash chromatography on silica gel using a mixture of CH2Cl2 and methanol (98:2) as the eluent. Yield: 1.30 g (57%).

후처리

  1. washthe solution was washed with water (3×25 ml), with a saturated aqueous solution of NaHCO3
  2. dry with materialdried (Na2SO4)
  3. customevaporated
  4. customThe product was purified by flash chromatography on silica gel using
  5. additiona mixture of CH2Cl2 and methanol (98:2) as the eluent

출처 및 근거

ORD 기록
ord-92bc942b064843acba5bd5d6358cfed0
출처 데이터셋
uspto-grants-1999_03
특허 번호
US05882628

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