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Hydrochloric Acid → HCID 25258315、化合物

HRID 422903
ノート
印刷プレビュー

反応式

HRID 422903 の反応式
[SH:1][CH2:2][CH:3]([CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([Br:14])[CH:9]=1)[C:4]([OH:6])=[O:5].Cl>CC(O)(C)C>[C:3]([S:1][CH2:2][CH:3]([CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([Br:14])[CH:9]=1)[C:4]([OH:6])=[O:5])([CH3:7])([CH3:4])[CH3:2]
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 313Hydrochloric AcidHCID 25258314HCID 25258314、化合物

生成物 1

HCID 25258315HCID 25258315、化合物

試薬・触媒・溶媒 1

HCID 6386tert-Butanol溶媒

実験手順

To the reaction mixture of step 5, under N2 atmosphere, was injected a mixture of t-BuOH (3 ml) and 37% HCl (2.5 ml). The reaction mixture was heated to reflux for 4 hours, then cooled to room temperature and partitioned between water and CH2Cl2. The combined CH2Cl2 phases were washed with brine, dried over sodium sulfate, filtered, and concentrated under reduced pressure. The crude product was purified by silica gel chromatography eluting with 0 to 5% EtOH in CH2Cl2 to give 2-(S-t-butylsulfanylmethyl)-3-(3-bromophenyl)propionic acid as a colorless, viscous oil, 0.133 g, 51%: HPLC purity: 94.5%, MS (ES−) [M−H+]: 329, 331.

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 4 hours
  3. custompartitioned between water and CH2Cl2
  4. washThe combined CH2Cl2 phases were washed with brine
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customThe crude product was purified by silica gel chromatography
  9. washeluting with 0 to 5% EtOH in CH2Cl2

出典と根拠

ORDレコード
ord-9c644f585f394612ab8ab8666f5e97e6
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08101665B2

反応ノート

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