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Hydrochloric Acid → HCID 25258315, 화합물

HRID 422903
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HRID 422903 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 25258314HCID 25258314, 화합물

생성물 1

HCID 25258315HCID 25258315, 화합물

시약·촉매·용매 1

HCID 6386tert-Butanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9c644f585f394612ab8ab8666f5e97e6
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08101665B2

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