4-[(2-Methylthio-ethyl)-(2-methoxy-benzoyl)-amino]-benzenesulfonamide → 4-[(2-Methylthio-ethyl)-(2-methoxy-benzyl)-amino]-benzenesulfonamide

HRID 1789659ノート

反応式

HRID 1789659 の反応式
B.C1COCC1.C1COCC1.[CH3:12][S:13][CH2:14][CH2:15][N:16]([C:27](=O)[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=1[O:34][CH3:35])[C:17]1[CH:22]=[CH:21][C:20]([S:23]([NH2:26])(=[O:25])=[O:24])=[CH:19][CH:18]=1>C1COCC1>[CH3:12][S:13][CH2:14][CH2:15][N:16]([CH2:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=1[O:34][CH3:35])[C:17]1[CH:18]=[CH:19][C:20]([S:23]([NH2:26])(=[O:24])=[O:25])=[CH:21][CH:22]=1

参加物

4

反応物 2

HCID 220362164-[(2-Methylthio-ethyl)-(2-methoxy-benzoyl)-amino]-benzenesulfonamideHCID 178419153HCID 178419153、化合物

生成物 1

HCID 220361674-[(2-Methylthio-ethyl)-(2-methoxy-benzyl)-amino]-benzenesulfonamide収率 77.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 1 M BH3.THF/THF (6.8 mL, 6.8 mmol) was added to a solution of 4-[(2-methylthio-ethyl)-(2-methoxy-benzoyl)-amino]-benzenesulfonamide (0.51 g, 1.34 mmol) in THF (5 mL). After 18 h, the excess BH3 was quenched by addition of 0.1 M HCl; followed by partitioning the mixture between CH2Cl2 and NaHCO3. The organic layer was dried (Na2SO4), filtered, evaporated in vacuo, and the residue was purified by MPLC (CH2Cl2 to 70:30 CH2Cl2/EtOAc) to afford 0.38 g (77%) of 4-[(2-methylthio-ethyl)-(2-methoxy-benzyl)-amino]-benzenesulfonamide as a clear glass.

後処理

  1. customthe excess BH3 was quenched by addition of 0.1 M HCl
  2. customby partitioning the mixture between CH2Cl2 and NaHCO3
  3. dry with materialThe organic layer was dried (Na2SO4)
  4. filtrationfiltered
  5. customevaporated in vacuo
  6. customthe residue was purified by MPLC (CH2Cl2 to 70:30 CH2Cl2/EtOAc)

出典と根拠

ORDレコード
ord-e17c250301514e26be8bfcb2abe5b00e
出典データセット
uspto-grants-2006_07
特許番号
US07071177B2

反応ノート

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