Hydrochloric Acid → 1093651-77-4

HRID 1876281ノート

反応式

HRID 1876281 の反応式
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

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 11776TriphenylphosphineHCID 516892Sodium BicarbonateHCID 86646305HCID 86646305、化合物

生成物 1

HCID 687009031093651-77-4

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bfbd51f075af45caa085ada2db1cd7c2
出典データセット
uspto-grants-2012_11
特許番号
US08309596B2

反応ノート

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