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Trimethylsilyldiazomethane → HCID 86669289, 화합물

HRID 2042806
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HRID 2042806 반응식
[CH3:1][Si](C=[N+]=[N-])(C)C.[Cl:8][C:9]1[CH:17]=[CH:16][C:12]([C:13]([OH:15])=[O:14])=[C:11]([O:18][CH2:19][CH:20]([F:22])[F:21])[N:10]=1>CO.C(Cl)Cl>[CH3:1][O:14][C:13](=[O:15])[C:12]1[CH:16]=[CH:17][C:9]([Cl:8])=[N:10][C:11]=1[O:18][CH2:19][CH:20]([F:21])[F:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 167693TrimethylsilyldiazomethaneHCID 82004536HCID 82004536, 화합물

생성물 1

HCID 86669289HCID 86669289, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

Trimethylsilyl diazomethane (2 M in hexane; 15.0 mL, 30.0 mmol) is added to a mixture of 6-chloro-2-(2,2-difluoro-ethoxy)-nicotinic acid (6.0 g, 25.3 mmol) in MeOH (50 mL) and DCM (100 mL). The reaction mixture is stirred at rt for 10 min, quenched with AcOH and concentrated. The residue is diluted with water and filtered. The filtercake is washed with water and dried at 40° C.

후처리

  1. customquenched with AcOH
  2. concentrationconcentrated
  3. additionThe residue is diluted with water
  4. filtrationfiltered
  5. washThe filtercake is washed with water
  6. customdried at 40° C.

출처 및 근거

ORD 기록
ord-dd8e0126a1ee4d858b9efa63586726e5
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08586604B2

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