Triethylamine → HCID 20448808, 화합물

HRID 358370

반응식

HRID 358370 반응식
[Si:1]([O:8][C@@H:9]1[CH2:13][C:12](=O)[CH:11]2[O:15][CH:10]12)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].[SH:16][CH2:17][CH2:18][CH2:19][CH2:20][OH:21].C(N(CC)CC)C.[Cl-].[NH4+]>CO>[Si:1]([O:8][CH:9]1[CH2:10][C:11](=[O:15])[C:12]([S:16][CH2:17][CH2:18][CH2:19][CH2:20][OH:21])=[CH:13]1)([C:4]([CH3:5])([CH3:6])[CH3:7])([CH3:2])[CH3:3]

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 25517Ammonium ChlorideHCID 5482614-Sulfanylbutan-1-olHCID 13362510HCID 13362510, 화합물

생성물 1

HCID 20448808HCID 20448808, 화합물수율 81%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

2.80 g (12.2 mmoles) of 4(R)-t-butyldimethylsilyloxy-2,3-epoxycyclopentanone and 1.30 g (12.2 mmoles) of 4-mercaptobutan-1-ol were dissolved in 12 ml of methanol, and with stirring 1.87 ml (13.5 mmoles) of triethylamine was added. The stirring was continued for 30 minutes. Ten milliliters of a saturated aqueous solution of ammonium chloride was added, and the mixture was concentrated. The residue was extracted with ethyl acetate, dried over anhydrous magnesium sulfate, filtered and concentrated. The resulting oily product was chromatographed on a silica gel column using hexane/ethyl acetate (8/1) as an eluent to give 3.12 g (81%) of 4(RS)-t-butyldimethylsilyloxy-2-(4-hydroxybutylthio)-2-cyclopentenone.

후처리

  1. additionwas added
  2. concentrationthe mixture was concentrated
  3. extractionThe residue was extracted with ethyl acetate
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe resulting oily product was chromatographed on a silica gel column

출처 및 근거

ORD 기록
ord-50b7a521cf9c4e52b702724c63423584
출처 데이터셋
uspto-grants-1984_08
특허 번호
US04466980

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