Methylamine → 4-bromo-N,3-dimethylbenzenesulfonamide

HRID 1023396ノート

反応式

HRID 1023396 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:8](Cl)(=[O:10])=[O:9])=[CH:4][C:3]=1[CH3:12].C[CH2:14][N:15](C(C)C)C(C)C.CN>CN(C)C=O.CO>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:15][CH3:14])(=[O:10])=[O:9])=[CH:4][C:3]=1[CH3:12]

参加物

6

反応物 3

HCID 6329MethylamineHCID 81531DiisopropylethylamineHCID 27375034-Bromo-3-methylbenzene-1-sulfonyl chloride

生成物 1

HCID 84680704-bromo-N,3-dimethylbenzenesulfonamide収率 69.2%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 4-bromo-3-methylbenzene-1-sulfonyl chloride (500 mg, 1.86 mmol) and DIEA (0.65 mL, 3.7 mmol) in N,N-dimethylformamide (5 mL) was added methylamine as a 2.0 M solution in methanol. The reaction mixture was allowed to stir at room temperature overnight. The reaction mixture was evaporated to dryness and was dissolved in dichloromethane (3 mL). The solution was washed with 1 N HCl (2×3 mL) and a saturated solution of NaHCO3 (3 mL). The organics were dried over Na2SO4 and evaporated to dryness to give 4-bromo-N,3-dimethylbenzenesulfonamide (340 mg).

後処理

  1. customThe reaction mixture was evaporated to dryness
  2. dissolutionwas dissolved in dichloromethane (3 mL)
  3. washThe solution was washed with 1 N HCl (2×3 mL)
  4. dry with materialThe organics were dried over Na2SO4
  5. customevaporated to dryness

出典と根拠

ORDレコード
ord-debb2f40ac054a8c93e42bc736d68535
出典データセット
uspto-grants-2014_05
特許番号
US08722704B2

反応ノート

読み込み中…