Water → HCID 19004087, 화합물

HRID 2225370노트

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HRID 2225370 반응식
[N:1]1([C:7]2[C:8]3[CH:21]=[CH:20][CH:19]=[CH:18][C:9]=3[CH2:10][C:11]3[CH:17]=[CH:16][CH:15]=[CH:14][C:12]=3[N:13]=2)[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.Br[CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH:17]1[C:11]2[CH2:10][C:9]3[CH:18]=[CH:19][CH:20]=[CH:21][C:8]=3[C:7]([N:1]3[CH2:2][CH2:3][N:4]([CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25])[CH2:5][CH2:6]3)=[N:13][C:12]=2[CH:14]=[CH:15][CH:16]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 1512464-(11H-Dibenz(b,e)azepin-6-yl)piperazine

생성물 1

HCID 19004087HCID 19004087, 화합물수율 80.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
70 °C

실험 절차

A mixture of 2.77 g of 6-(1-piperazinyl)-11H-dibenz[b,e]azepine, 2.00 g of ethyl bromoacetate and 1.38 g of potassium carbonate in 14 ml of N,N-dimethylformamide was stirred at 70° C. for 3 hrs. After cooling, water was added to the reaction mixture and extracted with ether. The etheral layer was washed with water, dried and concentrated. The residue was chromatographed on silica gel using a mixture of n-hexane and ethyl acetate (2:1 and 1:1) as eluents to give 2.91 g of colorless crystals, which were recrystallized from isopropyl ether to give colorless prisms, mp 107°-108° C.

후처리

  1. temperatureAfter cooling
  2. extractionextracted with ether
  3. washThe etheral layer was washed with water
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was chromatographed on silica gel using
  7. additiona mixture of n-hexane and ethyl acetate (2:1 and 1:1) as eluents

출처 및 근거

ORD 기록
ord-1a8d8680afc9476a9f54a3f6e587a316
출처 데이터셋
uspto-grants-1994_09
특허 번호
US05344828

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