Hydrochloric Acid → HCID 67148875, compound

HRID 2425854Notes

Reaction equation

HRID 2425854 reaction equation
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[CH:9]([C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([O:17][CH3:18])[C:12]=1[N+:19]([O-])=O)[OH:10].Cl.[Sn]>C(O)C>[NH2:19][C:12]1[C:13]([O:17][CH3:18])=[CH:14][CH:15]=[CH:16][C:11]=1[CH:9]([C:3]1[C:4]([F:8])=[CH:5][CH:6]=[CH:7][C:2]=1[F:1])[OH:10]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 5352426Tin atomHCID 67148212HCID 67148212, compound

Product 1

HCID 67148875HCID 67148875, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

13.3 g of (2,6-difluorophenyl)(3-methoxy-2-nitro-phenyl)methanol are dissolved in 75 ml of ethanol. At 0° C., 37 ml of concentrated hydrochloric acid (10 eq.) are slowly added to 10.5 g of tin (2.2 eq.) (exothermic reaction). After 18 hours, the ethanol is evaporated, the residue is taken up in ethyl acetate before being alkalinized with a 3N aqueous sodium hydroxide solution until the pH is close to 14. After decantation, the organic phase is dried over anhydrous sodium sulfate and concentrated in order to obtain 8.7 of the expected product.

Workup

  1. customthe ethanol is evaporated
  2. customis close to 14
  3. dry with materialAfter decantation, the organic phase is dried over anhydrous sodium sulfate
  4. concentrationconcentrated in order

Sources & evidence

ORD record
ord-2356103b5a124977a66a4752c097fafe
Source dataset
uspto-grants-2011_06
Patent number
US07968534B2

Reaction notes

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