Water → Ethyl 4-(2-Chlorodibenz[b,f][1,4]oxazepin-11-yl)-l-piperazineacetate

HRID 2225363

반응식

HRID 2225363 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:11][C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=3[N:8]=[C:7]([N:16]3[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]3)[C:6]=2[CH:22]=1.Br[CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:11][C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=3[N:8]=[C:7]([N:16]3[CH2:21][CH2:20][N:19]([CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26])[CH2:18][CH2:17]3)[C:6]=2[CH:22]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 2170AmoxapineHCID 7748Ethyl bromoacetateHCID 11430Potassium Carbonate

생성물 1

HCID 15224710Ethyl 4-(2-Chlorodibenz[b,f][1,4]oxazepin-11-yl)-l-piperazineacetate수율 72%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 3.4 g of 2-chloro-11-(1-piperazinyl)dibenz[b,f][1,4]oxazepine, 2.00 g of ethyl bromoacetate and 1.38 g of potassium carbonate in 16 ml of N,N-dimethylformamide was stirred at 60°-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 3.12 g of yellow crystals, which were recrystallized from n-hexane to give yellow prisms, mp 123°-123.5° 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-8acf82bddd3b40eb9a38a3cc50e542c7
출처 데이터셋
uspto-grants-1994_09
특허 번호
US05344828

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