Phosphonium, hexyltriphenyl-, bromide (1:1) → HCID 68818416, 화합물

HRID 732591

반응식

HRID 732591 반응식
[Br-].[CH2:2]([P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[CH2:3][CH2:4][CH2:5][CH2:6][CH3:7].CC(C)([O-])C.[K+].[C:33]([O:37][C:38]([N:40]1[CH2:44][C:43](=O)[CH2:42][C@@H:41]1[C@H:46]1[O:50][C:49]([CH3:52])([CH3:51])[N:48]([C:53](=[O:55])[CH3:54])[C@H:47]1[CH2:56][C:57]1[CH:62]=[C:61]([F:63])[CH:60]=[C:59]([F:64])[CH:58]=1)=[O:39])([CH3:36])([CH3:35])[CH3:34]>C1COCC1>[C:33]([O:37][C:38]([N:40]1[CH2:44]/[C:43](=[CH:2]\[CH2:3][CH2:4][CH2:5][CH2:6][CH3:7])/[CH2:42][C@@H:41]1[C@H:46]1[O:50][C:49]([CH3:51])([CH3:52])[N:48]([C:53](=[O:55])[CH3:54])[C@H:47]1[CH2:56][C:57]1[CH:58]=[C:59]([F:64])[CH:60]=[C:61]([F:63])[CH:62]=1)=[O:39])([CH3:36])([CH3:34])[CH3:35]

참가 물질

5

반응물 3

HCID 2724569Phosphonium, hexyltriphenyl-, bromide (1:1)HCID 23665647Potassium tert-butoxideHCID 68814480HCID 68814480, 화합물

생성물 1

HCID 68818416HCID 68818416, 화합물수율 76.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

Place under argon a suspension of n-hexyltriphenylphosphonium bromide (0.420 g, 1 mmol) in 10 mL of dry THF. Add potassium tert-butoxide (0.112 g, 1 mmol). Stir the mixture for 1 h. Add a solution of (R)-2-[(4S,5S)-3-Acetyl-4-(3,5-difluoro-benzyl)-2,2-dimethyl-oxazolidin-5-yl]-4-oxo-pyrrolidine-1-carboxylic acid tert-butyl ester (0.045 g, 0.1 mmol) in 5 mL of dry THF. Stir the mixture overnight. Add water, extract with diethyl ether, dry over MgSO4, concentrate under reduced pressure and purify (silica gel chromatography, eluting with ethyl ether:hexane mixtures) to give the title compound (0.04 g, 76%).

후처리

  1. stirringStir the mixture overnight
  2. extractionAdd water, extract with diethyl ether
  3. dry with materialdry over MgSO4
  4. concentrationconcentrate under reduced pressure
  5. custompurify
  6. wash(silica gel chromatography, eluting with ethyl ether:hexane mixtures)

출처 및 근거

ORD 기록
ord-2818c567f17b4da281a5882559522ab8
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07585885B2

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