Trimethylsilyldiazomethane → HCID 67080255, 화합물

HRID 1047994노트

반응식

HRID 1047994 반응식
[F:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]([C:14]([OH:16])=[O:15])[CH2:7][C:8]([CH3:13])([CH3:12])[O:9]2)=[CH:4][CH:3]=1.[Si](C=[N+]=[N-])(C)(C)[CH3:18]>C(Cl)Cl.CO>[F:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]([C:14]([O:16][CH3:18])=[O:15])[CH2:7][C:8]([CH3:13])([CH3:12])[O:9]2)=[CH:4][CH:3]=1

참가 물질

5

반응물 2

HCID 167693TrimethylsilyldiazomethaneHCID 670803947-fluoro-2,2-dimethyl-3,4-dihydro-2H-chromene-4-carboxylic acid

생성물 1

HCID 67080255HCID 67080255, 화합물수율 75.6%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

To 7-fluoro-2,2-dimethyl-3,4-dihydro-2H-chromene-4-carboxylic acid (0.280 g, 1.25 mmol) in CH2Cl2 (5 mL) and MeOH (1 mL) was added TMSCHN2 (0.937 mL, 1.87 mmol) dropwise. After the addition, the reaction was concentrated, loaded onto silica gel, and the product eluted using a gradient of 5% ethyl acetate/hexanes to 40% ethyl acetate/hexanes to provide the title compound (0.225 g, 75.6% yield).

후처리

  1. additionAfter the addition
  2. concentrationthe reaction was concentrated
  3. washthe product eluted

출처 및 근거

ORD 기록
ord-1044b212270e44d3be31a06de9b15704
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08569522B2

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