HCID 67809871, compound → HCID 131718273, compound

HRID 327154Notes

Reaction equation

HRID 327154 reaction equation
Cl.[N:2]1([CH2:7][CH2:8][C@@H:9]2[O:13][C@@H:12]([CH2:14][O:15][C:16]3[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][C:17]=3[Cl:24])[CH:11]=[CH:10]2)[CH:6]=[CH:5][N:4]=[CH:3]1>C(O)C>[ClH:24].[N:2]1([CH2:7][CH2:8][C@@H:9]2[O:13][C@H:12]([CH2:14][O:15][C:16]3[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][C:17]=3[Cl:24])[CH2:11][CH2:10]2)[CH:6]=[CH:5][N:4]=[CH:3]1

Participants

3

Reactant 1

HCID 67809871HCID 67809871, compound

Product 1

HCID 131718273HCID 131718273, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

In a vial, add ethanol (1 ml) to the product of Example 100 (0.050 g) and add PtO (0.025 g). Place a balloon filled with H2 gas over the mouth of the vial and stir overnight. Purify the resultant product on a silica column, eluting with CH2Cl2 →5% methanol/CH2Cl2. Add 0.1 N HCl (2 ml) to the resulting product and lyophilize to obtain the title compound, MS: m/z 339 (M+ +1).

Workup

  1. additionfilled with H2 gas over the mouth of the vial and
  2. customPurify the resultant product on a silica column
  3. washeluting with CH2Cl2 →5% methanol/CH2Cl2
  4. additionAdd 0.1 N HCl (2 ml) to the resulting product

Sources & evidence

ORD record
ord-8a156e36aca74f4f878dad3e2d4ecb9a
Source dataset
uspto-grants-1993_12
Patent number
US05272167

Reaction notes

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