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Hydrochloric Acid → HCID 53692438, 화합물

HRID 2270560
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HRID 2270560 반응식
[C:1]([O:5][C:6]([N:8]([C:22]([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:23])[CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([N+:16]([O-])=O)[C:11]=1[O:19][CH2:20][CH3:21])=[O:7])([CH3:4])([CH3:3])[CH3:2].[BH4-].[Na+].Cl.C(=O)([O-])O.[Na+]>O.O.O.O.O.O.[Ni](Cl)Cl.CO>[C:25]([O:24][C:22]([N:8]([C:6]([O:5][C:1]([CH3:2])([CH3:4])[CH3:3])=[O:7])[CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([NH2:16])[C:11]=1[O:19][CH2:20][CH3:21])=[O:23])([CH3:28])([CH3:26])[CH3:27]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 4311764Sodium borohydrideHCID 54256258HCID 54256258, 화합물

생성물 1

HCID 53692438HCID 53692438, 화합물수율 85%

시약·촉매·용매 2

HCID 11791229Dichloronickel;hexahydrate
촉매
HCID 887Methanol용매

실험 절차

To a mixture of the compound (5.09 g) obtained in Example 417d, nickel (II) chloride hexahydrate (61 mg) and methanol (130 ml), sodium borohydride (1.46 g) was added. The reaction mixture was stirred at room temperature for 20 min and, after addition of 2 N HCl, adjusted to pH 8 with a saturated aqueous sodium hydrogencarbonate solution and then concentrated under reduced pressure. To the resulting residue, water was added and the mixture was subjected to extraction with ethyl acetate. The organic layer was washed with a saturated aqueous sodium chloride solution, dried with anhydrous sodium sulfate and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent, ethyl acetate:n-hexane=1:4) to give the titled compound (yield, 85%).

후처리

  1. additionwas added
  2. concentrationconcentrated under reduced pressure
  3. additionTo the resulting residue, water was added
  4. extractionthe mixture was subjected to extraction with ethyl acetate
  5. washThe organic layer was washed with a saturated aqueous sodium chloride solution
  6. dry with materialdried with anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe resulting residue was purified by silica gel column chromatography (eluent, ethyl acetate:n-hexane=1:4)

출처 및 근거

ORD 기록
ord-7ee9e804d5354d07ab7fefdf92fd74cd
출처 데이터셋
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06331553B1

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