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Trifluoroacetic acid → HCID 67078130、化合物

HRID 1475648
ノート
印刷プレビュー

反応式

HRID 1475648 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 68170292HCID 68170292、化合物

生成物 1

HCID 67078130HCID 67078130、化合物収率 46.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-eab05b663895440e8afb02dda480e6f6
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09018258B2

反応ノート

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