Water → Laurolactam

Temperature

90 °C

In 500 mL three-necked flask equipped with a reflux condenser were placed 20 g of cyclododecanone oxime (Tokyo Chemical Industry Co., Ltd.), 0.13 g of zinc chloride and 80 g of toluene, and the mixture was heated to a temperature of 90° C. To the three-necked flask was added dropwise a solution of 0.28 g of cyanuric chloride dissolved in 30 g of toluene via a dropping funnel. Two hours after the end of dropping, the reaction solution was transferred to a 1 L separable flask equipped with a jacket. To the mixture was added 50 g of ultrapure water, and the mixture was stirred at a temperature of 80° C. for 15 min. After allowing the mixture to stand for 15 min, the aqueous layer was drained. Then, to the mixture was added 50 g of a 1% by weight aqueous solution of NaOH, and the mixture was stirred for 15 min. After allowing the mixture to stand for 15 min, the aqueous layer was drained. This operation was further conducted twice followed by addition of 50 g of ultrapure water, and then the mixture was stirred for 15 min. Then, the mixture was allowed to stand for 15 min, and an aqueous layer was drained. The reaction solution thus obtained was concentrated and a light transmittance difference (LT. diff) of laurolactam was determined to be 69.5%.

1. customIn 500 mL three-necked flask equipped with a reflux condenser
2. customTwo hours
3. customthe reaction solution was transferred to a 1 L separable flask
4. customequipped with a jacket
5. waitto stand for 15 min
6. stirringthe mixture was stirred for 15 min
7. waitto stand for 15 min
8. stirringthe mixture was stirred for 15 min
9. waitto stand for 15 min
10. customThe reaction solution thus obtained
11. concentrationwas concentrated

ORD record

ord-33cba0e7a8724a80bdd866993aa6c668

Source dataset

uspto-grants-2014_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08816069B2