1,4-Dioxane → HCID 13732377, 화합물

HRID 648488

반응식

HRID 648488 반응식
C1(O[C:8](=[O:30])[NH:9][C:10]2[CH:15]=[CH:14][C:13]([N:16]3[CH2:21][CH2:20][N:19]([C:22]4[CH:27]=[CH:26][C:25]([O:28][CH3:29])=[CH:24][CH:23]=4)[CH2:18][CH2:17]3)=[CH:12][CH:11]=2)C=CC=CC=1.C([N:33]([CH2:38][CH2:39][CH2:40][CH3:41])[CH2:34][C:35](O)=[O:36])C.O1CCOCC1>CN(C)C1C=CN=CC=1.O>[CH2:38]([N:33]1[CH2:34][C:35](=[O:36])[N:9]([C:10]2[CH:15]=[CH:14][C:13]([N:16]3[CH2:17][CH2:18][N:19]([C:22]4[CH:23]=[CH:24][C:25]([O:28][CH3:29])=[CH:26][CH:27]=4)[CH2:20][CH2:21]3)=[CH:12][CH:11]=2)[C:8]1=[O:30])[CH2:39][CH2:40][CH3:41]

참가 물질

6

반응물 3

HCID 312751,4-DioxaneHCID 981607Phenyl N-(4-(4-(4-methoxyphenyl)piperazin-1-yl)phenyl)carbamateHCID 22062329HCID 22062329, 화합물

생성물 1

HCID 13732377HCID 13732377, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 962Water용매

실험 절차

A mixture of 24 parts of phenyl[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]carbamate, 15.9 parts of ethyl N-butylglycine, 2 parts of N,N-dimethyl-4-pyridinamine and 200 parts of 1,4-dioxane was stirred and refluxed overnight. Then water was added and stirring was continued for a while. The reaction mixture was cooled, poured onto water and the whole was stirred. The precipitated product was filtered off, washed with water and dissolved in 150 parts of trichloromethane. This solution was stirred for 30 minutes with 3 parts of silica gel. The latter was filtered off and the filtrate was evaporated. The residue was crystallized from butanol. The product was filtered off and dried in vacuo at 60° C., yielding 2.3 parts of 1-butyl-3-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]-2,4-imidazolidinedione; mp. 183.7° C. (39).

후처리

  1. temperaturerefluxed overnight
  2. stirringstirring
  3. temperatureThe reaction mixture was cooled
  4. additionpoured onto water
  5. stirringthe whole was stirred
  6. filtrationThe precipitated product was filtered off
  7. washwashed with water
  8. dissolutiondissolved in 150 parts of trichloromethane
  9. stirringThis solution was stirred for 30 minutes with 3 parts of silica gel
  10. filtrationThe latter was filtered off
  11. customthe filtrate was evaporated
  12. customThe residue was crystallized from butanol
  13. filtrationThe product was filtered off
  14. customdried in vacuo at 60° C.

출처 및 근거

ORD 기록
ord-a58dcbe881a44734a4c7308289c6ecda
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04735942

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