Sodium sulfate decahydrate → HCID 56669765, 화합물

HRID 1817891노트

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HRID 1817891 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH:7]1([CH2:10][N:11]2[C:15]3[CH:16]=[CH:17][C:18]([S:20]([C:23]([CH3:29])([CH3:28])[C:24](OC)=[O:25])(=[O:22])=[O:21])=[CH:19][C:14]=3[N:13]=[C:12]2[CH2:30][C:31]([CH3:34])([CH3:33])[CH3:32])[CH2:9][CH2:8]1.[F-].[K+].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[CH:7]1([CH2:10][N:11]2[C:15]3[CH:16]=[CH:17][C:18]([S:20]([C:23]([CH3:28])([CH3:29])[CH2:24][OH:25])(=[O:22])=[O:21])=[CH:19][C:14]=3[N:13]=[C:12]2[CH2:30][C:31]([CH3:34])([CH3:33])[CH3:32])[CH2:8][CH2:9]1

참가 물질

6

반응물 4

HCID 62649Sodium sulfate decahydrateHCID 522689Potassium FluorideHCID 21226445Aluminium lithium hydrideHCID 59253268HCID 59253268, 화합물

생성물 1

HCID 56669765HCID 56669765, 화합물수율 93%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
0 °C

실험 절차

To a suspension of lithium aluminum hydride (37 mg, 0.98 mmol) in tetrahydrofuran (4 mL) was added a solution of methyl 2-{[1-(cyclopropylmethyl)-2-(2,2-dimethylpropyl)-1H-benzimidazol-5-yl]sulfonyl}-2-methylpropanoate (Step G, 400 mg, 0.98 mmol) in tetrahydrofuran (4 mL) at 0° C. After stirring for 3 h at 0° C., the mixture was quenched with potassium fluoride (170 mg, 2.96 mmol) and sodium sulfate decahydrate (1.26 g, 3.92 mmol) at 0° C., filtered through a pad of celite and concentrated. The resulting residue was purified by column chromatography on silica gel (hexane:ethyl acetate=1:1 as eluent) to afford the title compound (345 mg, 93%) as a white amorphous solid.

후처리

  1. filtrationfiltered through a pad of celite
  2. concentrationconcentrated
  3. customThe resulting residue was purified by column chromatography on silica gel (hexane:ethyl acetate=1:1 as eluent)

출처 및 근거

ORD 기록
ord-64a0671579aa4d92bffb772fbf4160f4
출처 데이터셋
uspto-grants-2009_10
특허 번호
US07598393B2

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