Water → HCID 12884177, compound

HRID 893972Notes

Reaction equation

HRID 893972 reaction equation
[NH:1]1[CH2:6][CH2:5][C:4](=[C:7]2[C:13]3=[N:14][CH:15]=[CH:16][CH:17]=[C:12]3[CH2:11][CH2:10][C:9]3[CH:18]=[CH:19][CH:20]=[CH:21][C:8]2=3)[CH2:3][CH2:2]1.O.[C:23](=O)([O:29]C(C)(C)C)[O:24][C:25]([CH3:28])([CH3:27])[CH3:26]>O1CCCC1>[C:23]([N:1]1[CH2:2][CH2:3][C:4](=[C:7]2[C:13]3=[N:14][CH:15]=[CH:16][CH:17]=[C:12]3[CH2:11][CH2:10][C:9]3[CH:18]=[CH:19][CH:20]=[CH:21][C:8]2=3)[CH2:5][CH2:6]1)([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:29]

Participants

5

Reactant 3

HCID 962WaterHCID 10039136HCID 10039136, compoundHCID 10219638Carbonic acid, bis(1,1-dimethylethyl) ester

Product 1

HCID 12884177HCID 12884177, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

Dissolve 13.8 g of 11-(4-piperidylidene)-6,11 dihydro-5H-benzo-[5,6]-cyclohepta-[1,2-b]-pyridine (Compound IC) prepared according to Villani et. al., J. Med. Chem. 15, 750 (1972) in 250 ml of dry tetrahydrofuran. With stirring, add in one portion 12 g of di-t-butyl carbonate and stir at room temperature overnight. The mixture is poured into water, is extracted with ether, is washed with water and the solvent removed. Recrystallize the residue from isopropyl ether. The melting point is 144°-145° C.

Workup

  1. customprepared
  2. stirringstir at room temperature overnight
  3. extractionis extracted with ether
  4. washis washed with water
  5. customthe solvent removed
  6. customRecrystallize the residue from isopropyl ether

Sources & evidence

ORD record
ord-86236355dae44ca6a962482efef8fca7
Source dataset
uspto-grants-1981_08
Patent number
US04282233

Reaction notes

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