HCID 15063398, compound → HCID 15063399, compound

HRID 641704Notes

Reaction equation

HRID 641704 reaction equation
[O:1]=[C:2]1[CH:14](C(OC(C)(C)C)=O)[N:6]2[C:7]3[C:12]([CH:13]=[C:5]2[CH2:4][CH2:3]1)=[CH:11][CH:10]=[CH:9][CH:8]=3>C1(C)C=CC=CC=1>[CH:11]1[CH:10]=[CH:9][CH:8]=[C:7]2[C:12]=1[CH:13]=[C:5]1[CH2:4][CH2:3][C:2](=[O:1])[CH2:14][N:6]12

Participants

3

Reactant 1

HCID 15063398HCID 15063398, compound

Product 1

HCID 15063399HCID 15063399, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

A solution of the crude product of Step 4 in 1.2 L of toluene was treated with 100 g of silica gel and the mixture was heated to reflux for 6 h. After cooling, the mixture was filtered and the filtrate was concentrated to give the title compound as a dark solid. 1H NMR (500 MHz, acetone-d6) δ 7.52 (d, 1H), 7.35 (d, 1H), 7.11 (t, 1H), 7.05 (t, 1H), 6.32 (s, 1H), 4.74 (s, 2H), 3.29 (m, 2H), 2.78 (m, 2H).

Workup

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 6 h
  3. temperatureAfter cooling
  4. filtrationthe mixture was filtered
  5. concentrationthe filtrate was concentrated

Sources & evidence

ORD record
ord-e392e63a13244083a8eaddf4c4934058
Source dataset
uspto-grants-2010_04
Patent number
US07696222B2

Reaction notes

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