Water → 2,3-Dihydro-2,2-dimethyl-7-benzofuranyl methyl(4-morpholinylthio)carbamate

HRID 435805

반응식

HRID 435805 반응식
[CH3:1][C:2]1([CH3:16])[O:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][C:8]=2[O:11][C:12]([NH:14][CH3:15])=[O:13])[CH2:3]1.[O:17]1[CH2:22][CH2:21][N:20]([S:23]Cl)[CH2:19][CH2:18]1.Cl.N1C=CC=CC=1.O>N1C=CC=CC=1>[CH3:15][N:14]([S:23][N:20]1[CH2:21][CH2:22][O:17][CH2:18][CH2:19]1)[C:12](=[O:13])[O:11][C:8]1[C:9]2[O:10][C:2]([CH3:16])([CH3:1])[CH2:3][C:4]=2[CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 2566CarbofuranHCID 10176127Pyridinium chlorideHCID 122977794-Morpholinesulfenyl chloride

생성물 1

HCID 413832,3-Dihydro-2,2-dimethyl-7-benzofuranyl methyl(4-morpholinylthio)carbamate수율 60.4%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A mixture of 6.6 g of carbofuran and 4.8 g of morpholinosulfenyl chloride in 40 ml of pyridine was allowed to stand at room temperature for about 18 hours. The mixture, which contained solid pyridine hydrochloride, was poured into water and the aqueous mixture extracted with diethyl ether. The ether extract was washed with dilute acid, then with water and with saturated sodium chloride solution and dried. Evaporation of the ether gave 6.1 g of 2,3-dihydro-2,2-dimethyl-7-benzofuranyl (methyl)(morpholinosulfenyl)carbamate, m.p. 75° -78° . Recrystallization from hexane-diethyl ether increased the melting point to 89° .

후처리

  1. extractionthe aqueous mixture extracted with diethyl ether
  2. extractionThe ether extract
  3. washwas washed
  4. additionwith dilute acid
  5. dry with materialwith water and with saturated sodium chloride solution and dried
  6. customEvaporation of the ether

출처 및 근거

ORD 기록
ord-68289026b5b44592bd76e0767cbb162a
출처 데이터셋
uspto-grants-1977_02
특허 번호
US04006231

연결된 노트

불러오는 중…