Potassium Carbonate → N,N'-Bis[(2,3-dihydroxypropyl)-2-hydroxyethyl]-5-[N-(2-hydroxyethyl)hydroxyacetamido]-2,4,6-triiodoisophthalamide

HRID 1461612

반응식

HRID 1461612 반응식
C([O:4][CH2:5][C:6]([NH:8][C:9]1[C:10]([I:39])=[C:11]([C:28]([NH:30][CH2:31][CH:32]([CH2:34][CH:35]([OH:38])[CH2:36][OH:37])[OH:33])=[O:29])[C:12]([I:27])=[C:13]([C:25]=1[I:26])[C:14]([NH:16][CH2:17][CH:18]([CH2:20][CH:21]([OH:24])[CH2:22][OH:23])[OH:19])=[O:15])=[O:7])(=O)C.C([O-])([O-])=O.[K+].[K+].[C:46](OCCBr)(=[O:48])[CH3:47]>CC(N(C)C)=O>[OH:24][CH:21]([CH2:22][OH:23])[CH2:20][CH:18]([OH:19])[CH2:17][NH:16][C:14](=[O:15])[C:13]1[C:25]([I:26])=[C:9]([N:8]([CH2:47][CH2:46][OH:48])[C:6](=[O:7])[CH2:5][OH:4])[C:10]([I:39])=[C:11]([C:28]([NH:30][CH2:31][CH:32]([CH2:34][CH:35]([OH:38])[CH2:36][OH:37])[OH:33])=[O:29])[C:12]=1[I:27]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 135641-Acetoxy-2-bromoethaneHCID 867453315-Acetoxyacetamido-N,N'-bis[(2,3-dihydroxypropyl)-2-hydroxyethyl]-2,4,6-triiodoisophthalamide

생성물 1

HCID 86745332N,N'-Bis[(2,3-dihydroxypropyl)-2-hydroxyethyl]-5-[N-(2-hydroxyethyl)hydroxyacetamido]-2,4,6-triiodoisophthalamide

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

실험 절차

5-Acetoxyacetamido-N,N'-bis[(2,3-dihydroxypropyl)-2-hydroxyethyl]-2,4,6-triiodoisophthalamide, prepared as in Example 3, Step B, (89 g, 0.1 g-mole) is mixed with K2CO3 (27.6 g, 0.2-g mole) and 2-bromoethyl acetate (33.4 g, 0.2 g-mole) in DMAc (200 ml). The mixture is stirred at 35°-40° C. until the reaction is complete (approximately 8-12 hours). The solution is then cooled to room temperature and the inorganic salts are filtered. The filtrate is then evaporated under vacuum at 70° C. to yield a thick oil. The oil is triturated with isopropyl alcohol to dissolve the residual DMAC and bromoethyl acetate. The supernatant is decanted and the residual solid is evaporated to dryness to provide the desired product.

후처리

  1. custom(approximately 8-12 hours)
  2. filtrationthe inorganic salts are filtered
  3. customThe filtrate is then evaporated under vacuum at 70° C.
  4. customto yield a thick oil
  5. customThe oil is triturated with isopropyl alcohol
  6. dissolutionto dissolve the residual DMAC and bromoethyl acetate
  7. customThe supernatant is decanted
  8. customthe residual solid is evaporated to dryness

출처 및 근거

ORD 기록
ord-d7decc12c099411e8ec205f3b0a56771
출처 데이터셋
uspto-grants-1991_12
특허 번호
US05075502

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