Dichloromethane → HCID 86660169, compound

HRID 1850316Notes

Reaction equation

HRID 1850316 reaction equation
C(OC([N:8]1[CH2:11][C:10]2([CH2:14][N:13]([C:15](=[O:17])[CH3:16])[CH2:12]2)[CH2:9]1)=O)(C)(C)C.C(O)(C(F)(F)F)=O.C(Cl)[Cl:26]>>[ClH:26].[CH2:12]1[C:10]2([CH2:11][NH:8][CH2:9]2)[CH2:14][N:13]1[C:15](=[O:17])[CH3:16]

Participants

4

Reactant 3

HCID 6344Dichloromethane2×HCID 6422Trifluoroacetic acidHCID 58547206HCID 58547206, compound

Product 1

HCID 86660169HCID 86660169, compoundYield 75%

Procedure

To a solution of 6-Acetyl-2,6-diaza-spiro[3.3]heptane-2-carboxylic acid tert-butyl ester (131) (300 mg, 1.33 mmol) in CH2Cl2 (10 mL) were added TFA (388 mg, 4.0 mmol). The reaction mixture was stirred at RT for 1 h, then diluted with CH2Cl2 (20 mL), washed with H2O (20 mL). The organic layer was washed with brine (20 mL), dried over Na2SO4, and filtered, evaporated to give the product (132) (176 mg, 1.0 mmol, yield: 75%). ESI-MS (M+1): 141 calc. for C7H12N2O 140.

Workup

  1. washwashed with H2O (20 mL)
  2. washThe organic layer was washed with brine (20 mL)
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. customevaporated

Sources & evidence

ORD record
ord-e2ee84d7c71e463bbae79a2458faed05
Source dataset
uspto-grants-2015_02
Patent number
US08957073B2

Reaction notes

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