HCID 20770232, compound → HCID 20770233, compound

HRID 1813883Notes

Reaction equation

HRID 1813883 reaction equation
[C:1]([O:4][C@@H:5]1[CH2:9][C@@H:8]([C@@H:10]([CH2:21][NH:22][C:23](=[O:39])[CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH3:38])[O:11]CC2C=CC(OC)=CC=2)[O:7][C@H:6]1[N:40]1[CH:45]=[CH:44][C:43](=[O:46])[NH:42][C:41]1=[O:47])(=[O:3])[CH3:2].C(Cl)Cl.FC(F)(F)C(O)=O>C(Cl)Cl.CCOCC>[C:1]([O:4][C@@H:5]1[CH2:9][C@@H:8]([C@@H:10]([CH2:21][NH:22][C:23](=[O:39])[CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH3:38])[OH:11])[O:7][C@H:6]1[N:40]1[CH:45]=[CH:44][C:43](=[O:46])[NH:42][C:41]1=[O:47])(=[O:3])[CH3:2]

Participants

5

Reactant 2

HCID 20770232HCID 20770232, compoundHCID 21863450Trifluoroacetic acid methylene chloride

Product 1

HCID 20770233HCID 20770233, compoundYield 24%

Reagents, catalysts & solvents 2

HCID 3283Diethyl EtherSolventHCID 6344DichloromethaneSolvent

Procedure

240 mg of the product of Stage A dissolved in 2 ml of methylene chloride is added to 7.5 ml of a mixture of methylene chloride/trifluoroacetic acid (9/1) under a nitrogen atmosphere. The solution obtained is agitated for 1 hour followed by evaporating and drying. A product is obtained which is taken up in ether then in pentane followed by evaporation again. The product obtained is chromatographed and 47 mg of sought product is obtained.

Workup

  1. customThe solution obtained
  2. customby evaporating
  3. customdrying
  4. customA product is obtained which
  5. customin pentane followed by evaporation again
  6. customThe product obtained
  7. customis chromatographed

Sources & evidence

ORD record
ord-2995e9cd92bd4beca533396e2336eca0
Source dataset
uspto-grants-2005_04
Patent number
US06875752B2

Reaction notes

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