Triphenylphosphine → HCID 20786265, compound

HRID 1392194Notes

Reaction equation

HRID 1392194 reaction equation
[OH:1][C:2]1[CH:26]=[CH:25][C:5]([CH2:6][C:7]23[CH2:14][CH2:13][CH2:12][N:11]2[C:10](=[O:15])[N:9]([C:16]2[CH:21]=[C:20]([Cl:22])[N:19]=[C:18]([Cl:23])[CH:17]=2)[C:8]3=[O:24])=[CH:4][CH:3]=1.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.O[CH2:47][CH2:48][C:49]1[CH:54]=[CH:53][N:52]=[CH:51][CH:50]=1.CCOC(/N=N/C(OCC)=O)=O>C(Cl)Cl>[N:52]1[CH:53]=[CH:54][C:49]([CH2:48][CH2:47][O:1][C:2]2[CH:3]=[CH:4][C:5]([CH2:6][C:7]34[CH2:14][CH2:13][CH2:12][N:11]3[C:10](=[O:15])[N:9]([C:16]3[CH:17]=[C:18]([Cl:23])[N:19]=[C:20]([Cl:22])[CH:21]=3)[C:8]4=[O:24])=[CH:25][CH:26]=2)=[CH:50][CH:51]=1

Participants

6

Reactant 4

HCID 11776TriphenylphosphineHCID 729214-PyridineethanolHCID 5462977Diethyl azodicarboxylateHCID 22479133HCID 22479133, compound

Product 1

HCID 20786265HCID 20786265, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

To a mixture of the compound from Example 196 (0.15 g), Ph3P (0.22 g) and 4-hydroxyethylpyridine ((0.070 mL) in anhydrous CH2Cl2 (3 mL) was added DEAD (0.15 mL) under N2. After 30 minutes the reaction mixture was concentrated and the residue was purified via HPLC to give the desired compound (97 mg). MS m/z 498(MH+).

Workup

  1. concentrationAfter 30 minutes the reaction mixture was concentrated
  2. customthe residue was purified via HPLC

Sources & evidence

ORD record
ord-709b4e6351914d588bdc3be1493bc2fd
Source dataset
uspto-grants-2008_03
Patent number
US07342012B2

Reaction notes

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