Ethanethiol → HCID 59948695, 화합물

HRID 651041노트

반응식

HRID 651041 반응식
[CH2:1]([SH:3])[CH3:2].[H-].[Na+].[CH:6]1([CH2:12][C@H:13]2[CH2:15][O:14]2)[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1.[NH4+].[Cl-]>CN(C=O)C>[CH:6]1([CH2:12][C@H:13]([OH:14])[CH2:15][S:3][CH2:1][CH3:2])[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1

참가 물질

6

반응물 4

HCID 6343EthanethiolHCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 59949024HCID 59949024, 화합물

생성물 1

HCID 59948695HCID 59948695, 화합물수율 81.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

Ethanethiol (317 μL, 4.3 mmol) was added to a 60% dispersion in mineral oil NaH (180 mg, 4.5 mmol) slurry in DMF (26 mL) at ambient temperature. After stirring for 15 minutes, the product from Example 15C (300 mg, 2.1 mmol) in DMF (2.0 mL) was added to the reaction vessel. After stirring for 30 minutes, a solution of saturated NH4Cl was added to the mixture followed by extraction with EtOAc (2×). The organics were combined, dried (MgSO4), and concentrated. The residue was chromatographed (silica gel; EtOAc/hexanes 1:20) to provide 347 mg (80%) of the title compound as a light yellow oil.

후처리

  1. stirringAfter stirring for 30 minutes
  2. extractionfollowed by extraction with EtOAc (2×)
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated
  5. customThe residue was chromatographed (silica gel; EtOAc/hexanes 1:20)

출처 및 근거

ORD 기록
ord-2c4534df552744e6b483ddf708c7c85a
출처 데이터셋
uspto-grants-2001_08
특허 번호
US06277871B1

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