Hydrochloric Acid → HCID 86761516, compound

HRID 1093417Notes

Reaction equation

HRID 1093417 reaction equation
C(OC(=O)[NH:7][C:8]1([CH2:16][CH2:17][C:18]2[CH:23]=[CH:22][C:21]([O:24][CH2:25][CH2:26][CH2:27][C:28]3[CH:29]=[C:30]4[C:34](=[CH:35][CH:36]=3)[C:33](=[O:37])[CH2:32][CH2:31]4)=[C:20]([C:38]([F:41])([F:40])[F:39])[CH:19]=2)[CH2:13][O:12]C(C)(C)[O:10][CH2:9]1)(C)(C)C.[ClH:43]>C(O)C>[ClH:43].[NH2:7][C:8]([CH2:16][CH2:17][C:18]1[CH:23]=[CH:22][C:21]([O:24][CH2:25][CH2:26][CH2:27][C:28]2[CH:29]=[C:30]3[C:34](=[CH:35][CH:36]=2)[C:33](=[O:37])[CH2:32][CH2:31]3)=[C:20]([C:38]([F:39])([F:40])[F:41])[CH:19]=1)([CH2:13][OH:12])[CH2:9][OH:10]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 59407785HCID 59407785, compound

Product 1

HCID 86761516HCID 86761516, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
80 °C

Procedure

Compound 56-4 (840 mg) was dissolved in ethanol (15 ml), concentrated hydrochloric acid (1.5 ml) was added, and the mixture was stirred at 80° C. for 1 hr. The reaction mixture was concentrated, and the residue was washed with diethyl ether to give a white powder. The white powder was purified by HPLC, the obtained residue was converted to hydrochloride by adding hydrogen chloride containing ether (1 mol/l, 15 ml), and the precipitate was collected by filtration and dried to give the object product (410 mg) as a white powder.

Workup

  1. concentrationThe reaction mixture was concentrated
  2. washthe residue was washed with diethyl ether
  3. customto give a white powder
  4. customThe white powder was purified by HPLC
  5. additionby adding hydrogen chloride
  6. additioncontaining ether (1 mol/l, 15 ml)
  7. filtrationthe precipitate was collected by filtration
  8. customdried

Sources & evidence

ORD record
ord-8d4eaebe289b4891832a52bb5ac8a3d9
Source dataset
uspto-grants-2012_03
Patent number
US08129361B2

Reaction notes

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