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Trifluoroacetic acid → HCID 67078130, 화합물

HRID 1475648
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HRID 1475648 반응식
[CH:1]1([CH:6]([C:14]2[CH:19]=[CH:18][C:17]([F:20])=[CH:16][CH:15]=2)[C:7]([O:9]C(C)(C)C)=[O:8])[CH2:5][CH2:4][CH2:3][CH2:2]1.FC(F)(F)C(O)=O>ClCCl>[CH:1]1([CH:6]([C:14]2[CH:19]=[CH:18][C:17]([F:20])=[CH:16][CH:15]=2)[C:7]([OH:9])=[O:8])[CH2:5][CH2:4][CH2:3][CH2:2]1
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참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 68170292HCID 68170292, 화합물

생성물 1

HCID 67078130HCID 67078130, 화합물수율 46.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2.20 g (about 88% pure, 6.96 mmol) of (+/−)-tert-butyl cyclopentyl(4-fluorophenyl)acetate were dissolved in 2.9 ml of dichloromethane, and 10.7 ml of trifluoroacetic acid were added at RT. The mixture was stirred at RT for 3 h and then concentrated under reduced pressure. The residue was dried under high vacuum overnight. The solid obtained was triturated with acetonitrile and then filtered off with suction and washed with a little acetonitrile. Drying under high vacuum gave 720 mg of a first solids batch. The filtrate obtained above was concentrated and the residue was purified by preparative RP-HPLC (mobile phase acetonitrile/water). This gave a further 529 mg of the target product (overall yield 80.8% of theory).

후처리

  1. concentrationconcentrated under reduced pressure
  2. customThe residue was dried under high vacuum overnight
  3. customThe solid obtained
  4. customwas triturated with acetonitrile
  5. filtrationfiltered off with suction
  6. washwashed with a little acetonitrile
  7. customDrying under high vacuum

출처 및 근거

ORD 기록
ord-eab05b663895440e8afb02dda480e6f6
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09018258B2

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