Tributylstannane → Benzopyran

HRID 487645

반응식

HRID 487645 반응식
C([C:3]1[CH:38]=[CH:37][C:6]2[O:7][C:8](C)(C)[CH:9]=[C:10](N3C=CC(C(OC(OC4C=CC=CC=4)=S)CC(OCC)=O)=CC3=O)[C:5]=2[CH:4]=1)#N.N(C(C)(C)C#N)=NC(C)(C)C#N.C([SnH](CCCC)CCCC)CCC>C1(C)C=CC=CC=1>[O:7]1[CH2:8][CH:9]=[CH:10][C:5]2[CH:4]=[CH:3][CH:38]=[CH:37][C:6]1=2

참가 물질

5

반응물 3

HCID 5948TributylstannaneHCID 6547AzobisisobutyronitrileHCID 217469106-cyano-2,2-dimethyl-4-{1,2-dihydro-2-oxo-4-(1-phenoxythiocarbonyloxy-2-ethoxycarbonylethyl)-1-pyridinyl}-2H-benzo[b]pyran

생성물 1

HCID 9211Benzopyran

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

In 3 ml of anhydrous toluene, is dissolved 73 mg of 6-cyano-2,2-dimethyl-4-{1,2-dihydro-2-oxo-4-(1-phenoxythiocarbonyloxy-2-ethoxycarbonylethyl)-1-pyridinyl}-2H-benzo[b]pyran obtained in Example 32. Then, 45 mg of 2,2'-azobisisobutyronitrile and 80 mg of tri-n-butyltin hydride are added to the solution at room temperature, and the resulting mixture is reacted at 100° C. for 30 minutes. After the reaction, the reaction mixture is directly purified by silica gel column chromatography to obtain 42 mg of 6-cyano-2,2-dimethyl-4-}-1,2-dihydro-2-oxo-4-(2-ethoxycarbonylethyl)-1pyridinyl}-2H-benzo[b]pyran.

후처리

  1. customthe resulting mixture is reacted at 100° C. for 30 minutes
  2. customAfter the reaction
  3. customthe reaction mixture is directly purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-d1e0c6ab5f8543d980db368112d94f4f
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05296492

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