Hydrochloric Acid → HCID 67905847, compound

HRID 1609053Notes

Reaction equation

HRID 1609053 reaction equation
[NH2:1][C@H:2]1[C@@H:6]([CH3:7])[CH2:5][N:4]([C:8]2[C:17]([F:18])=[CH:16][C:15]3[C:19](=[O:25])[C:20]([C:22]([OH:24])=[O:23])=[CH:21][N:13]4[C:14]=3[C:9]=2[CH2:10][CH2:11][N:12]4[CH3:26])[CH2:3]1.[ClH:27]>C(O)(=O)C>[ClH:27].[NH2:1][C@H:2]1[C@@H:6]([CH3:7])[CH2:5][N:4]([C:8]2[C:17]([F:18])=[CH:16][C:15]3[C:19](=[O:25])[C:20]([C:22]([OH:24])=[O:23])=[CH:21][N:13]4[C:14]=3[C:9]=2[CH2:10][CH2:11][N:12]4[CH3:26])[CH2:3]1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 9928823HCID 9928823, compound

Product 1

HCID 67905847HCID 67905847, compound

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

5.1 g of the compound (30) obtained in Example 5 (1) was dissolved in 110 ml of acetic acid, and then 25 ml of concentrated hydrochloric acid was added to the solution. The solution was stirred overnight at room temperature. The crystal was filtered off and washed successively with ethanol and ether to obtain 4.6 g of crude crystal. The filtrate was removed by distillation, and 80 ml of ethanol was added to the residue, and the deposited crystal was filtered off. The combined crude crystal was recrystallized from ethanol to obtain 4.61 g of the subject compound (77). The result of the analysis of this compound was as follows.

Workup

  1. filtrationThe crystal was filtered off
  2. washwashed successively with ethanol and ether
  3. customto obtain 4.6 g of crude crystal
  4. customThe filtrate was removed by distillation, and 80 ml of ethanol
  5. additionwas added to the residue
  6. filtrationthe deposited crystal was filtered off
  7. customThe combined crude crystal was recrystallized from ethanol

Sources & evidence

ORD record
ord-79b19215cf3349cc892caff7c5d1d5cd
Source dataset
uspto-grants-1995_03
Patent number
US05399553

Reaction notes

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