Dichloromethane → n-(3,3-Difluoro-cyclobutyl)-methanesulfonamide

HRID 1815459ノート

反応式

HRID 1815459 の反応式
Cl.[F:2][C:3]1([F:8])[CH2:6][CH:5]([NH2:7])[CH2:4]1.C(Cl)Cl.[CH3:12][S:13](Cl)(=[O:15])=[O:14]>C(N(CC)CC)C>[F:2][C:3]1([F:8])[CH2:6][CH:5]([NH:7][S:13]([CH3:12])(=[O:15])=[O:14])[CH2:4]1

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 31297Methanesulfonyl chlorideHCID 225009573,3-Difluorocyclobutamine hydrochloride

生成物 1

HCID 22500956n-(3,3-Difluoro-cyclobutyl)-methanesulfonamide

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

0.60 g 3,3-Difluoro-cyclobutylamine hydrochloride were suspended using 40 ml CH2Cl2 and 2.9 ml of triethylamine added at ambient temperature while receiving a clear solution. Thereafter, 1.0 ml of methanesulfonylchloride were added dropwise at ambient temperature and the mixture left at that temperature for 16 h. The volatiles were removed in vacuo, the residue was redissolved using 200 ml of EE and 100 ml of a saturated aqueous Na2CO3-solution and the layers separated. The organic layer was washed twice using 20 ml of a saturated aqueous NaHSO4-solution each time and washed twice using 30 ml of a saturated aqueous Na2CO3-solution each time. The organic layer was dried over MgSO4 and the solvent removed in vacuo. Yield: 700 mg of a colorless resin.

後処理

  1. additionadded at ambient temperature
  2. customThe volatiles were removed in vacuo
  3. dissolutionthe residue was redissolved
  4. customthe layers separated
  5. washThe organic layer was washed twice
  6. washwashed twice
  7. dry with materialThe organic layer was dried over MgSO4
  8. customthe solvent removed in vacuo

出典と根拠

ORDレコード
ord-295d0f2ee96e4c0eb2973b98f5c3fac2
出典データセット
uspto-grants-2005_04
特許番号
US06878748B2

反応ノート

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