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

HRID 1280133ノート

反応式

HRID 1280133 の反応式
[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]

参加物

5

反応物 2

HCID 6344DichloromethaneHCID 184291813-Hydroxymethyl-5-(2,3-dihydroxypropylaminocarbonyl)-2,4,6-triiodoaniline

生成物 1

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

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 7918Acetic Anhydride溶媒

実験手順

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.

後処理

  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
  5. additiona mixture of CH2Cl2 and methanol (98:2) as the eluent

出典と根拠

ORDレコード
ord-522a74c35ba24d1fb00e8f01597af576
出典データセット
uspto-grants-2002_09
特許番号
US06448442B1

反応ノート

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