Methanol → HCID 59470601, 화합물

HRID 219498

반응식

HRID 219498 반응식
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]

참가 물질

6

반응물 4

HCID 887MethanolHCID 31374DimethylacetamideHCID 134919PropanediolHCID 53903191HCID 53903191, 화합물

생성물 1

HCID 59470601HCID 59470601, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-9de2866bb0c1419ca7946ef3cf685deb
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08202511B2

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