Trifluoroacetic acid → HCID 58042402, 화합물

HRID 2048116노트

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HRID 2048116 반응식
[Cl:1][C:2]1[C:3]([O:16][C:17]2[CH:18]=[N:19][C:20]([CH:24]3[CH2:26][CH2:25]3)=[C:21]([Cl:23])[CH:22]=2)=[CH:4][C:5]([F:15])=[C:6]([CH:14]=1)[C:7]([O:9]C(C)(C)C)=[O:8].FC(F)(F)C(O)=O>ClCCl>[Cl:1][C:2]1[C:3]([O:16][C:17]2[CH:18]=[N:19][C:20]([CH:24]3[CH2:25][CH2:26]3)=[C:21]([Cl:23])[CH:22]=2)=[CH:4][C:5]([F:15])=[C:6]([CH:14]=1)[C:7]([OH:9])=[O:8]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 58042480HCID 58042480, 화합물

생성물 1

HCID 58042402HCID 58042402, 화합물수율 97%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
45 °C

실험 절차

To a solution of tert-butyl 5-chloro-4-[(5-chloro-6-cyclopropylpyridin-3-yl)oxy]-2-fluorobenzoate (Preparation 264, 54.0 g, 135.59 mmol) in dichloromethane (270 mL) was added trifluoroacetic acid (30.76 mL, 406.77 mmol). The resulting solution was heated at 45° C. for 24 hours and concentrated under reduced pressure at 45° C. tert Butyl methyl ether (100 mL) was added to the residue and the resulting slurry stirred at room temperature for 2.5 hours, filtered, washed with tert butyl methyl ether (20 mL) and dried to give the title compound as an off-white solid (45.0 g, 97%).

후처리

  1. concentrationconcentrated under reduced pressure at 45° C. tert Butyl methyl ether (100 mL)
  2. additionwas added to the residue
  3. filtrationfiltered
  4. washwashed with tert butyl methyl ether (20 mL)
  5. customdried

출처 및 근거

ORD 기록
ord-6aa7c4dcabb942ceb29551a63a210785
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08592629B2

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