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1,1',1''-Methanetriyltripiperidine → HCID 54010473, 화합물

HRID 2164323
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HRID 2164323 반응식
N1([CH:7]([N:14]2[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]2)N2CCCCC2)CCCCC1.[CH3:20][O:21][P:22]([NH:26][CH:27]1[C:34](=[O:35])[N:33]2[CH:28]1[S:29][CH2:30][C:31]([CH3:49])=[C:32]2[C:36]([O:38][CH2:39][C:40]1[CH:45]=[CH:44][C:43]([N+:46]([O-:48])=[O:47])=[CH:42][CH:41]=1)=[O:37])([O:24][CH3:25])=[O:23]>C(OCC)(=O)C>[CH3:20][O:21][P:22]([NH:26][CH:27]1[C:34](=[O:35])[N:33]2[CH:28]1[S:29][CH2:30][C:31]([CH:49]=[CH:7][N:14]1[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19]1)=[C:32]2[C:36]([O:38][CH2:39][C:40]1[CH:41]=[CH:42][C:43]([N+:46]([O-:48])=[O:47])=[CH:44][CH:45]=1)=[O:37])([O:24][CH3:25])=[O:23]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 126019201,1',1''-MethanetriyltripiperidineHCID 20406364HCID 20406364, 화합물

생성물 1

HCID 54010473HCID 54010473, 화합물수율 18.4%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

반응 조건

온도
45 °C

실험 절차

Tripiperidinomethane (1.06 g) is added to a solution of 7-dimethoxyphosphorylamino-3-methyl-2-(4-nitrobenzyloxycarbonyl)-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene (0.9 g) in ethyl acetate (40 cc) at 45° C., and the reaction mixture is stirred for 18 hours at 45° C. and diluted with ethyl acetate (20 cc). The organic solution is washed with distilled water (3×20 cc) and then with a saturated solution of sodium chloride (2×15 cc), dried over magnesium sulphate and concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 30° C. The residue obtained is recrystallised from ethyl acetate (5 cc), and 7-dimethoxyphosphorylamino-2-(4-nitrobenzyloxycarbonyl)-8-oxo-3-(2-piperidinovinyl)-5-thia-1-azabicyclo[4.2.0]oct-2-ene (E isomer) (0.2 g) is obtained in the form of an orange-yellow crystalline powder, m.p.=220°-221° C.

후처리

  1. washThe organic solution is washed with distilled water (3×20 cc)
  2. dry with materialwith a saturated solution of sodium chloride (2×15 cc), dried over magnesium sulphate
  3. concentrationconcentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 30° C
  4. customThe residue obtained
  5. customis recrystallised from ethyl acetate (5 cc)

출처 및 근거

ORD 기록
ord-e3462358719145afbe4f29ae38dd7cfb
출처 데이터셋
uspto-grants-1985_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04503220

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