Hydrochloric Acid → 3-[(2-Chloroacetyl)amino]-alpha-ethyl-2,4,6-triiodobenzenepropanoic acid

HRID 2258387

反応式

HRID 2258387 の反応式
[NH2:1][C:2]1[C:3]([I:17])=[C:4]([CH2:10][CH:11]([CH2:15][CH3:16])[C:12]([OH:14])=[O:13])[C:5]([I:9])=[CH:6][C:7]=1[I:8].[Cl:18][CH2:19][C:20](Cl)=[O:21].[OH-].[Na+].Cl>CC(N(C)C)=O.O>[Cl:18][CH2:19][C:20]([NH:1][C:2]1[C:3]([I:17])=[C:4]([CH2:10][CH:11]([CH2:15][CH3:16])[C:12]([OH:14])=[O:13])[C:5]([I:9])=[CH:6][C:7]=1[I:8])=[O:21]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 3735Iopanoic AcidHCID 6577Chloroacetyl chlorideHCID 14798Sodium Hydroxide

生成物 1

HCID 229213893-[(2-Chloroacetyl)amino]-alpha-ethyl-2,4,6-triiodobenzenepropanoic acid収率 95.3%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 31374Dimethylacetamide溶媒

実験手順

To a solution of 50 g of 3-amino-α-ethyl-2,4,6-triiodobenzenepropanoic acid (CAS RN, 96-83-3) (0.0875 mol) in 200 ml of DMA at 0° C., 11.87 g of chloroacetyl chloride (0.10 mol) are added. After 60 minutes at room temperature, the solution is dropwise added to 100 ml of H2O to give a precipitate which is filtered. The residue is dissolved in 100 ml of H2O and 43.7 ml of 2N NaOH (0.0875 mol) are added. 42 ml of 2N HCl (0.0084 mol) are added to precipitate a solid which is filtered. 5.4 g of 3-[(2-chloroacetyl)amino]-α-ethyl-2,4,6-triiodobenzenepropanoic acid are obtained (0.083 mol).

後処理

  1. customto give a precipitate which
  2. filtrationis filtered
  3. dissolutionThe residue is dissolved in 100 ml of H2O
  4. customto precipitate a solid which
  5. filtrationis filtered

出典と根拠

ORDレコード
ord-c5397c9c7a7348e9837ef19d496a2e9a
出典データセット
uspto-grants-1997_08
特許番号
US05660814

関連ノート

読み込み中…