Hydrochloric Acid → HCID 15547736, compound

HRID 1791119Notes

Reaction equation

HRID 1791119 reaction equation
[NH:1]1[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.Cl[CH2:8][C:9](=[O:15])[CH2:10][C:11]([O:13][CH3:14])=[O:12].O.Cl>ClCCl>[N:1]1([CH2:8][C:9](=[O:15])[CH2:10][C:11]([O:13][CH3:14])=[O:12])[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 8083MorpholineHCID 36240Methyl 4-chloroacetoacetate

Product 1

HCID 15547736HCID 15547736, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

1.27 g (14.6 mmol) of morpholine are added to a solution of 1.0 g (6.64 mmol) of methyl 4-chloroacetoacetate in 10 ml of dichloromethane, and the mixture is stirred at room temperature for 4 hours. Water is then added and the mixture is neutralized with 2N hydrochloric acid. The organic phase is dried over sodium sulfate and concentrated, and the residue is chromatographed on silica gel with cyclohexane/ethyl acetate (10:1→4:1→1:1) as mobile phase.

Workup

  1. dry with materialThe organic phase is dried over sodium sulfate
  2. concentrationconcentrated
  3. customthe residue is chromatographed on silica gel with cyclohexane/ethyl acetate (10:1→4:1→1:1) as mobile phase

Sources & evidence

ORD record
ord-66697104511a4a11a5a05a459f0b31cc
Source dataset
uspto-grants-2006_07
Patent number
US07074784B2

Reaction notes

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