Water → HCID 117600615, compound

HRID 1497703Notes

Reaction equation

HRID 1497703 reaction equation
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH2:8])=[C:4]([CH:9]([NH:16][CH3:17])[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH:3]=1.ClC(Cl)(O[C:22](=[O:28])OC(Cl)(Cl)Cl)Cl.O.CCOC(C)=O>C1COCC1>[Br:1][C:2]1[CH:3]=[C:4]2[C:5](=[CH:6][CH:7]=1)[NH:8][C:22](=[O:28])[N:16]([CH3:17])[CH:9]2[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

Participants

6

Reactant 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 94429TriphosgeneHCID 117600148HCID 117600148, compound

Product 1

HCID 117600615HCID 117600615, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

A solution of reactant 4-Bromo-2-(methylamino-phenyl-methyl)-phenylamine (3.4 g, 12 mmol) in THF (150 mL) is added triphosgene (3.81 g, 13 mmol). After the addition the mixture is stirred at r.t. for 3 h. Then H2O is added and is extacd with EtOAc, dried over Na2SO4 and concentrated. The residue is purified by chromatography on silica gel to give product.

Workup

  1. additionAfter the addition the mixture
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated
  4. customThe residue is purified by chromatography on silica gel
  5. customto give product

Sources & evidence

ORD record
ord-d2409f95c47d462cbfcdc6a9a592762b
Source dataset
uspto-grants-2015_12
Patent number
US09199988B2

Reaction notes

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