Triethylamine → HCID 23335655、化合物

N-(2-Hydroxypropyl)methacrylamide (7.15 g) was dissolved in dichloroethane (150 ml) in a 500 ml three-necked round-bottomed flask, fitted with a stirrer, two dropping funnels and a nitrogen supply. The flask was cooled to 0° C. by means of an ice/salt freezing mixture, stirring was started and the reaction was blanketed with dry nitrogen. `Topanol OC`, a butylated hydroxy toluene stabilizer, (0.1 g) was added. Tribromoacetylbromide (18 g) was added dropwise, simultaneously with triethylamine (5.1 g) over a period of 30 minutes, keeping the temperature between 0° and -5° C. While stirring the mixture was then slowly allowed to come to room temperature. After four hours the precipitated salts were filtered off, washed with dichloroethane, and the washings and filtrate were combined. The solvent was removed under vacuum by a rotary evaporator leaving an oil residue. This was dissolved in a mixture of water and ethanol and on standing the product crystallized as a colorless solid. It was recrystallized from the same solvent mixture. Yield (13 g) m.p. 104°-105° C.

1. customfitted with a stirrer
2. customthe temperature between 0° and -5° C
3. stirringWhile stirring the mixture
4. customto come to room temperature
5. filtrationAfter four hours the precipitated salts were filtered off
6. washwashed with dichloroethane
7. customThe solvent was removed under vacuum by a rotary evaporator
8. customleaving an oil residue
9. customcrystallized as a colorless solid
10. customIt was recrystallized from the same solvent mixture
11. customYield (13 g) m.p. 104°-105° C.

ORDレコード

ord-104828701e8a4302b9adbc6b85047474

出典データセット

uspto-grants-1980_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04229519