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Ammonium Chloride → 3-Ethyl-1,3,9,10,11,12-hexahydro-2H-quino[4,3,2-ef][1,4]benzoxazepin-2-one

HRID 1195781
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HRID 1195781 반응식
O.[NH2:2][C:3]1[C:4]2[C:9]([N:10]=[C:11]3[C:16]=1[CH2:15][CH2:14][CH2:13][CH2:12]3)=[CH:8][CH:7]=[CH:6][C:5]=2[O:17][CH:18]([CH2:24][CH3:25])[C:19](OCC)=[O:20].CC(C)([O-])C.[K+].[Cl-].[NH4+]>O1CCCC1>[CH2:24]([CH:18]1[C:19](=[O:20])[NH:2][C:3]2=[C:16]3[C:11](=[N:10][C:9]4=[CH:8][CH:7]=[CH:6][C:5](=[C:4]24)[O:17]1)[CH2:12][CH2:13][CH2:14][CH2:15]3)[CH3:25]
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참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 23665647Potassium tert-butoxideHCID 67757092Ethyl alpha-[(9-amino-1,2,3,4-tetrahydroacridin-8-yl)oxy]butyrate hydrate

생성물 1

HCID 537311453-Ethyl-1,3,9,10,11,12-hexahydro-2H-quino[4,3,2-ef][1,4]benzoxazepin-2-one수율 86%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of ethyl α-[(9-amino-1,2,3,4-tetrahydroacridin-8-yl)oxy]butyrate hydrate (30.34 g) in dry tetrahydrofuran (370 ml) was added potassium t-butoxide (13 g). The reaction mixture was stirred at room temperature for 1.5 hrs. Saturated ammonium chloride solution (150 ml) was added and stirring was continued for one hr. The mixture was concentrated and the concentrate was cooled. The solid was collected, washed with water, and dried to yield 21.26 g (78%) of product, mp 182°-183° C.

후처리

  1. stirringstirring
  2. waitwas continued for one hr
  3. concentrationThe mixture was concentrated
  4. temperaturethe concentrate was cooled
  5. customThe solid was collected
  6. washwashed with water
  7. customdried

출처 및 근거

ORD 기록
ord-c5efdc9e4f80423c80c6d8f12dfe425f
출처 데이터셋
uspto-grants-1992_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05112829

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