Hydrochloric Acid → 1093651-77-4

HRID 1876281노트

반응식

HRID 1876281 반응식
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[N:20]([CH2:23][C:24]1[C:33]2[C:28](=[CH:29][CH:30]=[C:31]([Cl:34])[CH:32]=2)[CH:27]=[CH:26][CH:25]=1)=[N+]=[N-].Cl.C([O-])(O)=O.[Na+]>C1COCC1.O>[ClH:34].[Cl:34][C:31]1[CH:32]=[C:33]2[C:28]([CH:27]=[CH:26][CH:25]=[C:24]2[CH2:23][NH2:20])=[CH:29][CH:30]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 11776TriphenylphosphineHCID 516892Sodium BicarbonateHCID 86646305HCID 86646305, 화합물

생성물 1

HCID 687009031093651-77-4

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

1.24 g of Triphenylphosphine and 410 μl of H2O are added to 998 mg of 1-azidomethyl-7-chloro-naphthalene in 20 ml of THF. The mixture obtained is stirred at 50° for 5 hours and solvent is evaporated. The residue obtained is acidified with aq. 1N HCl solution and extracted with EtOAc. The aq. phase obtained is basified with aq. 10% NaHCO3 solution and extracted with EtOAc. The organic phase obtained is dried and solvent is evaporated. The title compound is obtained as the free amine compound and converted to the hydrochloride salt by addition of 4M HCl solution in dioxane. Solvent is evaporated and the residue obtained is stirred with ether, the mixture obtained is filtered and the filtrate obtained is dried to yield the title compound.

후처리

  1. customThe mixture obtained
  2. customsolvent is evaporated
  3. customThe residue obtained
  4. extractionextracted with EtOAc
  5. customThe aq. phase obtained
  6. extractionextracted with EtOAc
  7. customThe organic phase obtained
  8. customis dried
  9. customsolvent is evaporated

출처 및 근거

ORD 기록
ord-bfbd51f075af45caa085ada2db1cd7c2
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08309596B2

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