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Acetone → HCID 70874615, 화합물

HRID 2172277
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HRID 2172277 반응식
C[O:2][C:3]1(OC)[CH2:8][CH2:7][N:6]([C:9]2[CH:28]=[CH:27][C:12]([O:13][CH2:14][C@@H:15]3[O:20][C:19]4=[N:21][C:22]([N+:24]([O-:26])=[O:25])=[CH:23][N:18]4[CH2:17][CH2:16]3)=[CH:11][CH:10]=2)[CH2:5][CH2:4]1.CC(C)=O.Cl>O>[N+:24]([C:22]1[N:21]=[C:19]2[N:18]([CH:23]=1)[CH2:17][CH2:16][C@H:15]([CH2:14][O:13][C:12]1[CH:11]=[CH:10][C:9]([N:6]3[CH2:5][CH2:4][C:3](=[O:2])[CH2:8][CH2:7]3)=[CH:28][CH:27]=1)[O:20]2)([O-:26])=[O:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 180AcetoneHCID 313Hydrochloric AcidHCID 86709411HCID 86709411, 화합물

생성물 1

HCID 70874615HCID 70874615, 화합물수율 99.5%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

(R)-7-[4-(4,4-Dimethoxypiperidin-1-yl)phenoxymethyl]-2-nitro-6,7-dihydro-5H-imidazo[2,1-b][1,3]oxazine (5.16 g), acetone (100 ml) and water (17 ml) were mixed. A 6 N hydrochloric acid aqueous solution (41 ml) was added thereto, followed by stirring at room temperature overnight. The reaction mixture was concentrated under reduced pressure. The remaining water layer was ice-cooled and neutralized by adding a 20% sodium carbonate aqueous solution. After being stirred at the same temperature for 10 minutes, the precipitated crystal was collected by filtration. The crystal thus obtained was dried at 60° C. to afford the title compound as a yellow solid (4.57 g).

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. temperaturecooled
  3. additionby adding a 20% sodium carbonate aqueous solution
  4. stirringAfter being stirred at the same temperature for 10 minutes
  5. filtrationthe precipitated crystal was collected by filtration
  6. customThe crystal thus obtained
  7. customwas dried at 60° C.

출처 및 근거

ORD 기록
ord-d7cdb82536bf4bff9b339cd68cedcc42
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09051333B2

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