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Dimethylamine → HCID 12952964, 화합물

HRID 2286237
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HRID 2286237 반응식
[ClH:1].[Cl:2][CH2:3][CH2:4][CH:5]1[CH2:9][N:8]([CH3:10])[C:7](=[NH:11])[N:6]1[CH3:12].[CH3:13][NH:14][CH3:15].C[OH:17]>>[OH2:17].[ClH:2].[ClH:1].[NH:11]=[C:7]1[N:6]([CH3:12])[CH:5]([CH2:4][CH2:3][N:14]([CH3:15])[CH3:13])[CH2:9][N:8]1[CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 674DimethylamineHCID 887MethanolHCID 20542259HCID 20542259, 화합물

생성물 1

HCID 12952964HCID 12952964, 화합물수율 26%

실험 절차

To 10.0 g (0.047 mole) of 4-(2-chloroethyl)-2-imino-1,3-dimethylimidazolidine hydrochloride was added 6.8 g (0.15 mole) of dimethylamine in 175 ml of methanol. The mixture was heated in a steel bomb at 100° C. for 15 hours. After concentrating in vacuo, the residue was partitioned between a dilute sodium carbonate solution and chloroform. The organic layer was dried (Na2SO4), filtered, and concentrated in vacuo. The residue was dissolved in ethyl acetate and treated with ethereal HCl. The hydrochloride was recrystallized from ethanol twice, and weighed 3.2 g (26% yield); m.p. 210°-212° C.

후처리

concentration
After concentrating in vacuo
  • customthe residue was partitioned between a dilute sodium carbonate solution and chloroform
  • dry with materialThe organic layer was dried (Na2SO4)
  • filtrationfiltered
  • concentrationconcentrated in vacuo
  • dissolutionThe residue was dissolved in ethyl acetate
  • additiontreated with ethereal HCl
  • customThe hydrochloride was recrystallized from ethanol twice
  • 출처 및 근거

    ORD 기록
    ord-bed42c60be7f4640a6f36472818164b8
    출처 데이터셋
    uspto-grants-1982_04
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04327107

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