Hydrochloric Acid → N,N-dimethyl-N-(4-nitrophenyl)carbamylmethyl-N-3-aminopropylammonium chloride

HRID 1973211노트

반응식

HRID 1973211 반응식
[Cl-:1].[CH3:2][N+:3]([CH3:23])([CH2:10][C:11](=[O:22])[NH:12][C:13]1[CH:18]=[CH:17][C:16]([N+:19]([O-:21])=[O:20])=[CH:15][CH:14]=1)[CH2:4][CH2:5][CH2:6][NH:7]C=O.Cl.[OH-].[Na+]>O>[Cl-:1].[CH3:23][N+:3]([CH3:2])([CH2:10][C:11](=[O:22])[NH:12][C:13]1[CH:18]=[CH:17][C:16]([N+:19]([O-:21])=[O:20])=[CH:15][CH:14]=1)[CH2:4][CH2:5][CH2:6][NH2:7]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 86733006N,N-dimethyl-N-(4-nitrophenyl)carbamylmethyl-N-3-formamidopropylammonium chloride

생성물 1

HCID 86733010N,N-dimethyl-N-(4-nitrophenyl)carbamylmethyl-N-3-aminopropylammonium chloride

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of 10.0 parts of N,N-dimethyl-N-(4-nitrophenyl)carbamylmethyl-N-3-formamidopropylammonium chloride in 100 parts of water containing 6.0 parts of concentrated hydrochloric acid was heated for about two hours. The reaction mixture was rendered slightly alkaline by the addition of 50 percent aqueous sodium hydroxide and stored in the refrigerator for two days. The reaction mixture was then filtered to remove a small amount of solid and the filtrate was acidified with 48 parts of concentrated hydrochloric acid. Acetone was slowly added to the acidified filtrate until precipitation started. When precipitation of the product was complete, the solid was collected on a filter, washed with acetone, and dried at 75° C. to obtain 8.2 parts of N,N-dimethyl-N-(4-nitrophenyl)carbamylmethyl-N-3-aminopropylammonium chloride as the mono-hydrochloride salt, a white solid which melted at 244°-245° C.

후처리

  1. filtrationThe reaction mixture was then filtered
  2. customto remove a small amount of solid
  3. additionAcetone was slowly added to the acidified filtrate until precipitation
  4. customWhen precipitation of the product
  5. customthe solid was collected on a filter
  6. washwashed with acetone
  7. customdried at 75° C.

출처 및 근거

ORD 기록
ord-4154e928244d47feb8ac0591a8416a6c
출처 데이터셋
uspto-grants-1976_12
특허 번호
US03996282

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