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Aziridine → HCID 20373424, 화합물

HRID 259046
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HRID 259046 반응식
[NH2:1][CH2:2][CH2:3][CH:4]1[CH2:9][CH2:8][CH:7]([CH2:10][CH2:11][NH2:12])[CH2:6][CH2:5]1.[CH2:13]1[NH:15][CH2:14]1.[Cl-].[NH4+]>>[NH2:15][CH2:14][CH2:13][NH:1][CH2:2][CH2:3][CH:4]1[CH2:9][CH2:8][CH:7]([CH2:10][CH2:11][NH2:12])[CH2:6][CH2:5]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 9033AziridineHCID 25517Ammonium ChlorideHCID 140298721,4-Cyclohexanediethanamine

생성물 1

HCID 20373424HCID 20373424, 화합물

실험 절차

1,4-Bis-(2-aminoethyl)cyclohexane (68 gm., 0.4 mole) and ethyleneimine (4.3 gm., 0.1 mole) with 0.4 g. ammonium chloride is mixed in a glasslined pressure reactor and filled with nitrogen to 100 psi. The mixture is shaken and heated to 85°-95° C. for 48 hours. After cooling, it is distilled rapidly free of the salt and then fractionated under high vacuum. The starting diamine is readily distinguished from the triamine product by thin layer chromatography and silica gel using a mixture of 1 volume concentrated aqueous ammonium hydroxide with 4 volume methyl alcohol, the diamine having a much higher Rf.

후처리

  1. additionfilled with nitrogen to 100 psi
  • temperatureheated to 85°-95° C. for 48 hours
  • temperatureAfter cooling
  • distillationit is distilled rapidly free of the salt
  • additiona mixture of 1 volume concentrated aqueous ammonium hydroxide with 4 volume methyl alcohol
  • 출처 및 근거

    ORD 기록
    ord-41a72292c7664ec8b7a8aa38b661ef5d
    출처 데이터셋
    uspto-grants-1977_07
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04035174

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