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

HRID 1789659노트

반응식

HRID 1789659 반응식
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

참가 물질

4

반응물 2

HCID 220362164-[(2-Methylthio-ethyl)-(2-methoxy-benzoyl)-amino]-benzenesulfonamideHCID 178419153HCID 178419153, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-e17c250301514e26be8bfcb2abe5b00e
출처 데이터셋
uspto-grants-2006_07
특허 번호
US07071177B2

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