Water → 3,4-difluoro-N-methylbenzene-1-sulfonamide

HRID 1964593ノート

反応式

HRID 1964593 の反応式
[F:1][C:2]1[CH:3]=[C:4]([S:9](Cl)(=[O:11])=[O:10])[CH:5]=[CH:6][C:7]=1[F:8].Cl.CN.[CH2:16]([N:18](CC)CC)C.O>ClCCl>[F:1][C:2]1[CH:3]=[C:4]([S:9]([NH:18][CH3:16])(=[O:11])=[O:10])[CH:5]=[CH:6][C:7]=1[F:8]

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 27369133,4-Difluorobenzene-1-sulfonyl chlorideHCID 6364545Methylamine hydrochloride

生成物 1

HCID 84679853,4-difluoro-N-methylbenzene-1-sulfonamide収率 30%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Commercially available 3,4-difluorophenylsulfonylchloride (117 μL, 0.87 mmol) was dissolved in dichloromethane (5 mL), and methylamine hydrochloride (49 mg, 0.73 mmol) and triethylamine (203 μL, 1.45 mmol) were added, followed by stirring at room temperature for 2 hours. To the reaction solution, water (15 mL) was added, extraction was carried out twice with dichloromethane (15 mL), and washing was carried out with saturated brine (15 mL), followed by drying over sodium sulfate. The solvent was distilled off under reduced pressure, followed by vacuum drying, to afford the desired compound (44.7 mg, yield 30%) as a colorless oil.

後処理

  1. extractionextraction
  2. washwashing
  3. dry with materialby drying over sodium sulfate
  4. distillationThe solvent was distilled off under reduced pressure
  5. customdrying

出典と根拠

ORDレコード
ord-82d86fa2c9cc4f4897aab3ac305771ba
出典データセット
uspto-grants-2013_04
特許番号
US08415359B2

反応ノート

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