Methane → HCID 21161941, 화합물

HRID 893954

반응식

HRID 893954 반응식
[Cl:1][CH2:2][C:3]([N:5]=[C:6]=[O:7])=[O:4].C1(C)C=CC=CC=1.[C:15]([CH:17]1[CH2:19][NH:18]1)#[N:16].C>C(OCC)(=O)C>[Cl:1][CH2:2][C:3]([NH:5][C:6]([N:18]1[CH2:19][CH:17]1[C:15]#[N:16])=[O:7])=[O:4]

참가 물질

6

반응물 4

HCID 297MethaneHCID 1140Toluene2회HCID 78209Chloroacetyl isocyanateHCID 118115Aziridine-2-carbonitrile

생성물 1

HCID 21161941HCID 21161941, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A solution of 36 g. chloroacetyl isocyanate in 100 ml. toluene is added dropwise, while stirring and cooling, at a temperature of 20° to 30° C. to 20.4 g. 2-cyanoaziridine dissolved in 200 ml. toluene. The resulting suspension is further stirred for 1 hour at ambient temperature, then filtered with suction. The solid material obtained is washed with toluene and triturated with diethyl ether to give 62 g. of crude product. This is introduced into about 2.5 to 3 liters ethyl acetate at a temperature of 60° C., boiled for a short time and the clear solution treated with active charcoal. After filtration, the clear and still hot filtrate is evaporated in a vacuum and the evaporation residue is triturated with anhydrous diethyl ether and dried for 1 hour at 70° C. There are obtained 39.3 g. of product with a melting point of 152°-155° C. After further purification by stirring for 5 minutes with 200 ml. ethyl acetate at 60° C. and trituration of the crystals obtained with diethyl ether, there are obtained, after drying in a vacuum at 70° C. 28.9 g. 1-(N-chloroacetyl-carbamoyl)-2-cyanoaziridine; m.p. 152°-155° C.

후처리

  1. temperaturecooling, at a temperature of 20° to 30° C. to 20.4 g
  2. stirringThe resulting suspension is further stirred for 1 hour at ambient temperature
  3. filtrationfiltered with suction
  4. customThe solid material obtained
  5. washis washed with toluene
  6. customtriturated with diethyl ether
  7. customto give 62 g
  8. filtrationAfter filtration
  9. customthe clear and still hot filtrate is evaporated in a vacuum
  10. customthe evaporation residue is triturated with anhydrous diethyl ether
  11. customdried for 1 hour at 70° C
  12. customThere are obtained 39.3 g
  13. customAfter further purification
  14. stirringby stirring for 5 minutes with 200 ml
  15. customethyl acetate at 60° C. and trituration of the crystals obtained with diethyl ether, there
  16. customare obtained
  17. customafter drying in a vacuum at 70° C

출처 및 근거

ORD 기록
ord-95d1922f260b4e2488e5cae8440755bc
출처 데이터셋
uspto-grants-1981_08
특허 번호
US04282212

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