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

HRID 2258387

반응식

HRID 2258387 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 31374Dimethylacetamide용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-c5397c9c7a7348e9837ef19d496a2e9a
출처 데이터셋
uspto-grants-1997_08
특허 번호
US05660814

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