Hydrochloric Acid → HCID 21449345, 화합물

HRID 597064

반응식

HRID 597064 반응식
Cl.[Cl:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([N:13]([C:17]3[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[CH:19][CH:18]=3)[N:14]=CC)=[N:8][CH:9]=[N:10]2)=[CH:5][CH:4]=1.Cl>C(O)C>[Cl:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([N:13]([C:17]3[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[CH:19][CH:18]=3)[NH2:14])=[N:8][CH:9]=[N:10]2)=[CH:5][CH:4]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 86734555acetaldehyde N1-(7-chloroquinazolin-4-yl)p-methoxyphenylhydrazone hydrochloride

생성물 1

HCID 21449345HCID 21449345, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A suspension of acetaldehyde N1 -(7-chloroquinazolin-4-yl)-p-methoxyphenylhydrazone hydrochloride (15.0g.) in ethanol (120ml.; dried over magnesium ethoxide) was cooled and stirred at 5°-10° C for 3 hrs. during the passage of dry hydrogen chloride. The mixture was then left at 0°-5° C. for 3 days before separation by filtration. The solid was washed with dry ether (10ml.), and then dissolved in a mixture of water (30ml.), saturated sodium acetate solution (5ml.) and ethyl acetate (25ml.). The aqueous layer was extracted with more ethyl acetate (2 × 15ml.), and the extracts washed with water (20ml.), dried (Na2SO4) and evaporated to give N1 -(7-chloroquinazolin-4-yl)-p-methoxyphenylhydrazine, m.p. 124°-127° C.

후처리

  1. temperaturewas cooled
  2. waitThe mixture was then left at 0°-5° C. for 3 days before separation by filtration
  3. washThe solid was washed with dry ether (10ml.)
  4. dissolutiondissolved in a mixture of water (30ml.), saturated sodium acetate solution (5ml.) and ethyl acetate (25ml.)
  5. extractionThe aqueous layer was extracted with more ethyl acetate (2 × 15ml.)
  6. washthe extracts washed with water (20ml.)
  7. dry with materialdried (Na2SO4)
  8. customevaporated

출처 및 근거

ORD 기록
ord-5bc2e9d69aee48f691891766db751553
출처 데이터셋
uspto-grants-1977_03
특허 번호
US04012513

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