Triethylamine → t-butyl N-chlorothio-N-methylcarbamate

HRID 1633170

반응식

HRID 1633170 반응식
[S:1]([Cl:3])Cl.[CH3:4][NH:5][C:6](=[O:12])[O:7][C:8]([CH3:11])([CH3:10])[CH3:9].C(N(CC)CC)C>C(Cl)Cl>[Cl:3][S:1][N:5]([CH3:4])[C:6](=[O:12])[O:7][C:8]([CH3:11])([CH3:10])[CH3:9]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 25353Sulfur dichlorideHCID 527635tert-Butyl methylcarbamate

생성물 1

HCID 13367233t-butyl N-chlorothio-N-methylcarbamate수율 103.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
5 °C

실험 절차

To a solution of 62 g (0.6 mole) of sulfur dichloride in 200 ml of methylene chloride cooled to 0° C. under a nitrogen atmosphere was added a solution made up of 50.9 g (0.4 mole) of t-butyl N-methylcarbamate, 44.5 g (0.44 mole) of triethylamine and 100 ml of methylene chloride. The temperature was maintained at -2° to 5° C. during the addition. After stirring for one additional hour at 5° C., the mixture was filtered under a positive nitrogen atmosphere, and the filtrate was concentrated. Solid was removed by extracting the product with hexane. After filtration the hexane solution was concentrated to give 81.5 g of t-butyl N-chlorothio-N-methylcarbamate.

후처리

  1. additionwas added a solution
  2. temperatureThe temperature was maintained at -2° to 5° C. during the addition
  3. filtrationthe mixture was filtered under a positive nitrogen atmosphere
  4. concentrationthe filtrate was concentrated
  5. customSolid was removed
  6. extractionby extracting the product with hexane
  7. filtrationAfter filtration the hexane solution
  8. concentrationwas concentrated

출처 및 근거

ORD 기록
ord-e53766b730974d15ada2f85fb895bd2e
출처 데이터셋
uspto-grants-1984_10
특허 번호
US04479002

연결된 노트

불러오는 중…