Ethanol hydrochloride → HCID 77244194, compound

HRID 1022571Notes

Reaction equation

HRID 1022571 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[O:14][CH2:13][CH2:12][N:11](C(OC(C)(C)C)=O)[CH2:10][CH:9]2[CH2:22][OH:23])=[CH:4][C:3]=1[F:24].Cl.C(O)C>>[ClH:1].[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[O:14][CH2:13][CH2:12][NH:11][CH2:10][CH:9]2[CH2:22][OH:23])=[CH:4][C:3]=1[F:24]

Participants

3

Reactant 2

HCID 21887872Ethanol hydrochloride2×HCID 66975800HCID 66975800, compound

Product 1

HCID 77244194HCID 77244194, compoundYield 154.9%

Procedure

To tert-butyl (6RS,7SR)-7-(4-chloro-3-fluorophenyl)-6-(hydroxymethyl)-1,4-oxazepane-4-carboxylate (229 mg) was added 2 N hydrogen chloride-ethanol solution (1.02 ml), and the mixture was stirred at room temperature for 1 hr. Further, 14.7 N hydrogen chloride-ethanol solution (2 mL) was added, and the mixture was stirred for 10 min. The oil obtained by concentration under reduced pressure was crystallized from diisopropyl ether-ethanol to give the title compound (146 mg).

Workup

  1. stirringthe mixture was stirred for 10 min
  2. customThe oil obtained by concentration under reduced pressure
  3. customwas crystallized from diisopropyl ether-ethanol

Sources & evidence

ORD record
ord-45995d037c4f4ac49a82867e02d8cbbb
Source dataset
uspto-grants-2014_05
Patent number
US08722662B2

Reaction notes

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