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

HRID 1613027

反応式

HRID 1613027 の反応式
IC1C(C(N)=O)=C(I)C=C(I)[C:3]=1[C:4](N)=[O:5].C([O:19][CH2:20][C:21]([NH:23][C:24]1[C:25]([I:54])=[C:26]([C:43]([NH:45][CH2:46][CH:47]([CH2:49][CH:50]([OH:53])[CH2:51][OH:52])[OH:48])=[O:44])[C:27]([I:42])=[C:28]([C:40]=1[I:41])[C:29]([NH:31][CH2:32][CH:33]([CH2:35][CH:36]([OH:39])[CH2:37][OH:38])[OH:34])=[O:30])=[O:22])(=O)C.C([O-])([O-])=O.[K+].[K+].C(OCCBr)(=O)C>CC(N(C)C)=O>[OH:39][CH:36]([CH2:37][OH:38])[CH2:35][CH:33]([OH:34])[CH2:32][NH:31][C:29](=[O:30])[C:28]1[C:40]([I:41])=[C:24]([N:23]([CH2:3][CH2:4][OH:5])[C:21](=[O:22])[CH2:20][OH:19])[C:25]([I:54])=[C:26]([C:43]([NH:45][CH2:46][CH:47]([CH2:49][CH:50]([OH:53])[CH2:51][OH:52])[OH:48])=[O:44])[C:27]=1[I:42]

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 135641-Acetoxy-2-bromoethaneHCID 221238242,4,6-TriiodoisophthalamideHCID 867453315-Acetoxyacetamido-N,N'-bis[(2,3-dihydroxypropyl)-2-hydroxyethyl]-2,4,6-triiodoisophthalamide

生成物 1

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

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

5[N-(2-Acetoxyethyl)acetoxyacetamido]-N,N'-bis(2,3-dihydroxypropyl)-2-hydroxyethyl]-2,4,6-triiodoisophthalamide. 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.

後処理

  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

出典と根拠

ORDレコード
ord-154df0e7a90240068f454989b404beaa
出典データセット
uspto-grants-1993_03
特許番号
US05191120

関連ノート

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