Water → 5-Chloroacetamido-2,4,6-triiodoisophthalic acid dichloride

HRID 894304

反応式

HRID 894304 の反応式
[Cl:1][CH2:2][C:3](Cl)=[O:4].[NH2:6][C:7]1[C:8]([I:21])=[C:9]([C:18]([Cl:20])=[O:19])[C:10]([I:17])=[C:11]([C:15]=1[I:16])[C:12]([Cl:14])=[O:13].O>CC(N(C)C)=O>[Cl:1][CH2:2][C:3]([NH:6][C:7]1[C:15]([I:16])=[C:11]([C:12]([Cl:14])=[O:13])[C:10]([I:17])=[C:9]([C:8]=1[I:21])[C:18]([Cl:20])=[O:19])=[O:4]

参加物

5

反応物 3

HCID 962WaterHCID 6577Chloroacetyl chlorideHCID 98948585-Amino-2,4,6-triiodoisophthaloyl dichloride

生成物 1

HCID 223545415-Chloroacetamido-2,4,6-triiodoisophthalic acid dichloride収率 75%

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

At maximally 10° C., 67.7 g (0.6 mol) of chloroacetyl chloride is added dropwise under agitation within 20 minutes to a solution of 119.1 g (0.2 mol) of 5-amino-2,4,6-triiodoisophthalic acid dichloride in 400 ml of dimethylacetamide; the mixture is further stirred for 1 hour under ice cooling and then overnight at room temperature. The reaction mixture is then treated with 6 l of water, the thus-produced precipitate is vacuum-filtered and dissolved in 3.5 l of ethyl acetate. The ethyl acetate solution is washed neutral with 400 ml of saturated NaHCO3 solution and twice with water, dried with Na2SO4, and concentrated under vacuum. The residue is treated with 800 ml of ether and dried under vacuum at 50° C., thus obtaining 100.8 g (75% of theory) of 5-chloroacetamido-2,4,6-triiodoisophthalic acid dichloride, m.p. 254°-256° C. (decomposition).

後処理

  1. customovernight
  2. customat room temperature
  3. filtrationthe thus-produced precipitate is vacuum-filtered
  4. dissolutiondissolved in 3.5 l of ethyl acetate
  5. washThe ethyl acetate solution is washed neutral with 400 ml of saturated NaHCO3 solution and twice with water
  6. dry with materialdried with Na2SO4
  7. concentrationconcentrated under vacuum
  8. additionThe residue is treated with 800 ml of ether
  9. customdried under vacuum at 50° C.

出典と根拠

ORDレコード
ord-8eebf5c88c2a44b3aa586ade7085d2e5
出典データセット
uspto-grants-1981_08
特許番号
US04283381

関連ノート

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