Hydrogen Bromide → HCID 12319449, compound

HRID 1077327Notes

Reaction equation

HRID 1077327 reaction equation
C[O:2][C:3]1[CH:16]=[C:15]2[C:6]([CH:7]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[O:8][C:9]32[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]3)=[CH:5][CH:4]=1.Br>>[OH:2][C:3]1[CH:16]=[C:15]2[C:6]([CH:7]([C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=3)[O:8][C:9]32[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]3)=[CH:5][CH:4]=1

Participants

3

Reactant 2

HCID 260Hydrogen BromideHCID 12319448HCID 12319448, compound

Product 1

HCID 12319449HCID 12319449, compound

Procedure

A suspension of 2.0 g. of 1,3-dihydro-6-methoxy-3-phenylspiro[isobenzofuran-1,4'-piperidine], (Example 73), and 32 ml. of a 48% hydrobromic acid solution is heated at reflux, effecting the separation of a hydrobromide salt as a crystalline precipitate. The mixture is poured into ice-water with stirring, the precipitate collected by filtration, the filter cake washed with water, and dried. Recrystallization from ethanol gives colorless crystals, m.p. 274°-276°, dec.

Workup

  1. additionA suspension of 2.0 g
  2. temperatureat reflux
  3. customthe separation of a hydrobromide salt as a crystalline precipitate
  4. additionThe mixture is poured into ice-water
  5. filtrationthe precipitate collected by filtration
  6. washthe filter cake washed with water
  7. customdried
  8. customRecrystallization from ethanol
  9. customgives colorless crystals, m.p. 274°-276°, dec.

Sources & evidence

ORD record
ord-9e5dba1375c9485cb83a988132eaafdf
Source dataset
uspto-grants-1976_05
Patent number
US03959475

Reaction notes

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