Dichloromethane → Diethylamino-sulfenyl carbamoyl fluoride

HRID 26950

反応式

HRID 26950 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 131711024Diethylamino-sulfenyl carbamoyl fluoride収率 62.9%

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-169c72cf116c4a2a91821603167f86f8
出典データセット
uspto-grants-1979_04
特許番号
US04151353

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