Calcium Carbonate → HCID 86602379, compound

HRID 1348501Notes

Reaction equation

HRID 1348501 reaction equation
[ClH:1].Cl.[NH2:3][C:4]1[CH:9]=[C:8]([NH2:10])[CH:7]=[C:6]([CH3:11])[C:5]=1[O:12][CH3:13].[C:14](=[O:17])([O-:16])[O-].[Ca+2].Cl[C:20]([O:22][CH2:23][CH2:24][Cl:25])=[O:21].O1[CH2:31][CH2:30]OCC1>>[CH3:13][O:12][C:5]1[C:6]([CH3:11])=[CH:7][C:8]([NH:10][C:14](=[O:17])[O:16][CH2:30][CH2:31][Cl:1])=[CH:9][C:4]=1[NH:3][C:20](=[O:21])[O:22][CH2:23][CH2:24][Cl:25]

Participants

5

Reactant 4

HCID 10112Calcium CarbonateHCID 123052-Chloroethyl chloroformateHCID 312751,4-DioxaneHCID 20389417HCID 20389417, compound

Product 1

HCID 86602379HCID 86602379, compound

Conditions

Temperature
90 °C

Procedure

56 g of 2,4-diamino-6-methylanisole dihydrochloride and 134 g of calcium carbonate were initially introduced into 1 l of dioxane and heated to 90° C. Within 15 min, 80 g of 2-chloroethyl chloroformate were added and the mixture was stirred for a further 4 h at this temperature. Subsequently, the mixture was left to cool, and the mineral salts were filtered off. The filtrate was poured onto iced water, and the mixture was extracted several times with ethyl acetate. The combined ethyl acetate phases were then evaporated to dryness on a Rotavapor, giving pale brown crystals.

Workup

  1. waitSubsequently, the mixture was left
  2. temperatureto cool
  3. filtrationthe mineral salts were filtered off
  4. additionThe filtrate was poured onto iced water
  5. extractionthe mixture was extracted several times with ethyl acetate
  6. customThe combined ethyl acetate phases were then evaporated to dryness on a Rotavapor
  7. customgiving pale brown crystals

Sources & evidence

ORD record
ord-1218509bf7364d2ebeac4cecb4929ad8
Source dataset
uspto-grants-2007_05
Patent number
US07211119B2

Reaction notes

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