Methanol → HCID 59470601、化合物

HRID 219498

反応式

HRID 219498 の反応式
Cl[C:2]([C:4]1[C:5]([I:24])=[C:6]([N:15]([CH3:23])[C:16]([CH2:18][O:19][C:20](=[O:22])[CH3:21])=[O:17])[C:7]([I:14])=[C:8]([C:11]([Cl:13])=[O:12])[C:9]=1[I:10])=[O:3].[CH:25]([OH:29])(O)[CH2:26][CH3:27].C[OH:31].C[C:33]([N:35](C)C)=O>C(OCC)(=O)C>[Cl:13][C:11]([C:8]1[C:7]([I:14])=[C:6]([N:15]([CH3:23])[C:16]([CH2:18][O:19][C:20](=[O:22])[CH3:21])=[O:17])[C:5]([I:24])=[C:4]([C:2](=[O:3])[N:35]([CH2:27][CH:26]([OH:31])[CH2:25][OH:29])[CH3:33])[C:9]=1[I:10])=[O:12]

参加物

6

反応物 4

HCID 887MethanolHCID 31374DimethylacetamideHCID 134919PropanediolHCID 53903191HCID 53903191、化合物

生成物 1

HCID 59470601HCID 59470601、化合物

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

Acetic acid [(3,5-bis-chlorocarbonyl-2,4,6-triiodo-phenyl)-methyl-carbamoyl]-methyl ester (16.25 g, 22.9 mmol) and 3-methylamino-1,2,-propanediol (4.42 ml, 45.8 mmol) were stirred in DMA (80 ml) for 72 hours at room temperature. The mixture was diluted with ethyl acetate (150 ml) and washed with ice water/brine (50:50, 20 ml×3). The organics were collected, dried over MgSO4, filtered and evaporated to dryness. The product was purified by silica column chromatography eluting with DCM: methanol to give acetic acid ({3-chlorocarbonyl-5-[(2,3-dihydroxy-propyl)-methyl-carbamoyl]-2,4,6-triiodo-phenyl}-methyl-carbamoyl)-methyl ester (5.42 g, 6.96 mmol).

後処理

  1. washwashed with ice water/brine (50:50, 20 ml×3)
  2. customThe organics were collected
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. customevaporated to dryness
  6. customThe product was purified by silica column chromatography
  7. washeluting with DCM

出典と根拠

ORDレコード
ord-9de2866bb0c1419ca7946ef3cf685deb
出典データセット
uspto-grants-2012_06
特許番号
US08202511B2

関連ノート

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