Dichloromethane → HCID 86756309, compound

HRID 567666Notes

Reaction equation

HRID 567666 reaction equation
Cl.[NH2:2][C:3]1C(C)=[CH:6][S:5][C:4]=1[C:9]([O:11][CH:12]([CH3:14])[CH3:13])=[O:10].[CH2:15]([Cl:17])[Cl:16].C(=O)(O)[O-].[Na+]>O>[ClH:16].[NH2:2][C:3]1[C:15]([Cl:17])=[CH:6][S:5][C:4]=1[C:9]([O:11][CH:12]([CH3:14])[CH3:13])=[O:10]

Participants

5

Reactant 3

HCID 6344DichloromethaneHCID 516892Sodium BicarbonateHCID 86756311HCID 86756311, compound

Product 1

HCID 86756309HCID 86756309, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

11.75 g (50 mmol) of i-propyl 3-amino-4-methyl-thiophene-2-carboxylate hydrochloride are dissolved in 100 ml of water. 150 ml of methylene chloride are added to this solution, and sodium bicarbonate is then added a little at a time until a pH of 7 has been exceeded. The mixture is stirred for 8 hours and the organic phase is separated off, washed with water, dried with magnesium sulphate and filtered. The filtrate is concentrated using water pump vacuum and the amorphous residue is crystallized from petroleum ether.

Workup

  1. additionis then added a little at a time until a pH of 7
  2. customthe organic phase is separated off
  3. washwashed with water
  4. dry with materialdried with magnesium sulphate
  5. filtrationfiltered
  6. concentrationThe filtrate is concentrated
  7. customthe amorphous residue is crystallized from petroleum ether

Sources & evidence

ORD record
ord-7dfd0c70b65d474d9193aec5bbf55486
Source dataset
uspto-grants-2001_01
Patent number
US06180567B2

Reaction notes

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