Hydrochloric Acid → HCID 66685052、化合物

HRID 714245ノート

反応式

HRID 714245 の反応式
[F:1][C:2]1[CH:3]=[C:4]([C:9]2(/[CH:15]=[CH:16]/[C:17]([O:19]CC)=[O:18])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]2)[CH:5]=[CH:6][C:7]=1[F:8].[OH-].[Na+].Cl>CO>[F:1][C:2]1[CH:3]=[C:4]([C:9]2(/[CH:15]=[CH:16]/[C:17]([OH:19])=[O:18])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]2)[CH:5]=[CH:6][C:7]=1[F:8]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 86688201(E)-ethyl 3-(1-(3,4-difluorophenyl)cyclohexyl)acrylate

生成物 1

HCID 66685052HCID 66685052、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of (E)-ethyl 3-(1-(3,4-difluorophenyl)cyclohexyl)acrylate (Preparation Int. 3-C, 53 mg, 0.180 mmol) in MeOH (1 mL) was added 1M NaOH (0.216 mL, 0.216 mmol), and the mixture was stirred at room temperature overnight. The mixture was acidified by the addition of 0.3 mL of 1N HCl, and the product was extracted with EtOAc. The extract was washed with brine, dried over Na2SO4 and evaporated to give the (E)-3-(1-(3,4-difluorophenyl)cyclohexyl)acrylic acid as an oil. 1H NMR (400 MHz, CDCl3) δ ppm 11.94 (1 H, br. s.), 7.11 (2 H, m), 7.02 (1H, d, J=15.82 Hz), 6.98-7.06 (1H, m), 5.62 (1 H, d, J=15.82 Hz), 1.83-2.06 (4 H, m), 1.37-1.65 (6 H, m).

後処理

  1. extractionthe product was extracted with EtOAc
  2. washThe extract was washed with brine
  3. dry with materialdried over Na2SO4
  4. customevaporated

出典と根拠

ORDレコード
ord-b7d7f0a566784228a0890d9c2352ee63
出典データセット
uspto-grants-2015_11
特許番号
US09187437B2

反応ノート

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