Acetic Anhydride → HCID 15132482, compound

HRID 1089185

Reaction equation

HRID 1089185 reaction equation
[CH2:1]1[C:6]2([CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]2)[CH2:5][CH2:4][NH:3][CH2:2]1.[C:12](OC(=O)C)(=[O:14])[CH3:13]>O1CCCC1>[C:12]([N:3]1[CH2:4][CH2:5][C:6]2([CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]2)[CH2:1][CH2:2]1)(=[O:14])[CH3:13]

Participants

4

Reactant 2

HCID 7918Acetic AnhydrideHCID 4174123-Azaspiro(5.5)undecane hydrochloride

Product 1

HCID 15132482HCID 15132482, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

A solution of 7 ml of 3-azaspiro[5.5]undecane and 9.7 ml of acetic anhydride in 19.5 ml of tetrahydrofuran was refluxed for 3 hours. The volatiles were evaporated to a yellow oil which was distilled in a Kugelrohr still giving a yellow oil, BP 90°-100° C./200-atm. The distillate was purified by chromatography on silica gel using 1:1 ethyl acetate:hexanes giving 7.89 g of the desired product as a colorless oil.

Workup

  1. customThe volatiles were evaporated to a yellow oil which
  2. distillationwas distilled in a Kugelrohr
  3. customstill giving a yellow oil, BP 90°-100° C./200-atm
  4. distillationThe distillate was purified by chromatography on silica gel using 1:1 ethyl acetate

Sources & evidence

ORD record
ord-d318633b5f464a62b74f0062febe4b8e
Source dataset
uspto-grants-1990_10
Patent number
US04965284

Linked notes

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