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Hydrochloric Acid → HCID 10388100、化合物

HRID 1883272
ノート
印刷プレビュー

反応式

HRID 1883272 の反応式
C([O:3][C:4](=[O:33])/[C:5](/[F:32])=[C:6](\[CH3:31])/[CH:7]=[CH:8]/[C:9](/[F:30])=[C:10](\[C:12]1[C:21]([O:22][CH2:23][CH2:24][CH3:25])=[CH:20][C:19]2[C:18]([CH3:27])([CH3:26])[CH2:17][CH2:16][C:15]([CH3:29])([CH3:28])[C:14]=2[CH:13]=1)/[CH3:11])C.[OH-].[Na+].Cl>CCO>[F:32]/[C:5](=[C:6](/[CH3:31])\[CH:7]=[CH:8]\[C:9](\[F:30])=[C:10](/[C:12]1[C:21]([O:22][CH2:23][CH2:24][CH3:25])=[CH:20][C:19]2[C:18]([CH3:27])([CH3:26])[CH2:17][CH2:16][C:15]([CH3:29])([CH3:28])[C:14]=2[CH:13]=1)\[CH3:11])/[C:4]([OH:33])=[O:3]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 12146419(2Z,4E,6E)-2,6-difluoro-3-methyl-7-(5,5,8,8-tetramethyl-3-propoxy-5,6,7,8-tetrahydro-naphthalen-2-yl)-octa-2,4,6-trienoic acid ethyl ester2 回

生成物 1

HCID 10388100HCID 10388100、化合物収率 73%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
60 °C

実験手順

To a solution of (2Z,4E,6E)-2,6-difluoro-3-methyl-7-(5,5,8,8-tetramethyl-3-propoxy-5,6,7,8-tetrahydro-naphthalen-2-yl)-octa-2,4,6-trienoic acid ethyl ester (Compound 10, 82 mg, 0.18 mmol) in EtOH (2 mL) was added 1M NaOH (1.0 mL). The mixture was heated to 60° C. for 2 h and was cooled to ambient temperature, acidified with 1M HCl, and extracted with EtOAc (×3). The combined organic layer was washed with brine, dried over Na2SO4, and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel (50% EtOAc-hexane) to give the title compound as a pale yellow solid (56 mg, 73%).

後処理

  1. temperaturewas cooled to ambient temperature
  2. extractionextracted with EtOAc (×3)
  3. washThe combined organic layer was washed with brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by flash column chromatography on silica gel (50% EtOAc-hexane)

出典と根拠

ORDレコード
ord-91b6ab371c2744079bd8cdf87f73c26e
出典データセット
uspto-grants-2004_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06759547B1

反応ノート

読み込み中…

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