Dichloromethane → Diethylamino-sulfenyl carbamoyl fluoride

HRID 26950

반응식

HRID 26950 반응식
[FH:1].C(Cl)Cl.C[N:6]=[C:7]=[O:8].[CH2:9]([N:11]([CH2:14][CH3:15])[S:12]Cl)[CH3:10]>C(N(CC)CC)C>[CH2:9]([N:11]([CH2:14][CH3:15])[S:12][NH:6][C:7]([F:1])=[O:8])[CH3:10]

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 12228Methyl IsocyanateHCID 14917Hydrofluoric AcidHCID 12297776N,N-diethylaminosulfenyl chloride

생성물 1

HCID 131711024Diethylamino-sulfenyl carbamoyl fluoride수율 62.9%

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

Anhydrous hydrogen fluoride (3.0 g, 0.15 mole) was added to 150 ml of methylene chloride at -10° C. Then 8.6 g of methylisocyanate was added, followed by 20.9 g (0.15 mole) of N,N-diethylaminosulfenyl chloride at 0° C. Triethylamine (15.2 g) was then added at 0° C. over a 15-minute period, and the mixture was stirred at +5° C. for 1 hour. The mixture was then extracted with water (100 ml), saturated sodium bicarbonate solution, and water again. After drying (MgSO4), the solvent was removed in vacuo, and the crude residue was vacuum distilled to give 17 g of N-methyl-N-(diethylamino-sulfenyl carbamoyl fluoride, b.p. 57° C./0.8 mm (62.9 percent yield).

후처리

  1. extractionThe mixture was then extracted with water (100 ml), saturated sodium bicarbonate solution, and water again
  2. dry with materialAfter drying (MgSO4)
  3. customthe solvent was removed in vacuo
  4. distillationdistilled

출처 및 근거

ORD 기록
ord-169c72cf116c4a2a91821603167f86f8
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04151353

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