Tetraethyltin → 7-Ethyl-5-nitro-1,3-benzothiazole

HRID 1489132노트

반응식

HRID 1489132 반응식
Br[C:2]1[C:10]2[S:9][CH:8]=[N:7][C:6]=2[CH:5]=[C:4]([N+:11]([O-:13])=[O:12])[CH:3]=1.[CH2:14]([Sn](CC)(CC)CC)[CH3:15]>CCOC(C)=O>[CH2:14]([C:2]1[C:10]2[S:9][CH:8]=[N:7][C:6]=2[CH:5]=[C:4]([N+:11]([O-:13])=[O:12])[CH:3]=1)[CH3:15]

참가 물질

4

반응물 2

HCID 11704TetraethyltinHCID 227280317-Bromo-5-nitrobenzothiazole

생성물 1

HCID 227280367-Ethyl-5-nitro-1,3-benzothiazole수율 75.9%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

A solution of 7-bromo-5-nitrobenzothiazole (0.15 g, 0.58 mmol), tetraethyltin (0.18 mL, 0.87 mmol) and catalytic amount of Cl2 Pd(PPh3)2 in a sealed tube was stirred for 12 h at 90° C. The reaction mixture was diluted with EtOAc and washed with brine several times. Organic solution was dried over Na2SO4 and concentrated in vacuo, yielding an oil which was subjected to column chromatography (EtOAc, neat) to provide 91 mg (0.44 mmol, 75%) of the desired product.

후처리

  1. washwashed with brine several times
  2. dry with materialOrganic solution was dried over Na2SO4
  3. concentrationconcentrated in vacuo
  4. customyielding an oil which

출처 및 근거

ORD 기록
ord-98013f6c225846cc946819d9a2d8a790
출처 데이터셋
uspto-grants-1997_10
특허 번호
US05677321

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