Triacetoxyperiodinane → HCID 49820158, 화합물

HRID 1914786노트

반응식

HRID 1914786 반응식
[OH:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][CH:8]=[C:7]([C:10]([C:12]3[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][CH:13]=3)=[O:11])[C:6]=2[CH:20]=1.CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=[O:23].C(Cl)(Cl)Cl.CO>CS(C)=O>[CH3:19][O:18][C:15]1[CH:16]=[CH:17][C:12]([C:10]([C:7]2[C:6]3[C:20](=[O:23])[C:2](=[O:1])[CH:3]=[CH:4][C:5]=3[O:9][CH:8]=2)=[O:11])=[CH:13][CH:14]=1

참가 물질

5

반응물 3

HCID 159087TriacetoxyperiodinaneHCID 687117(5-hydroxy-1-benzofuran-3-yl)(4-methoxyphenyl)methanoneHCID 21584188Chloroform methanol

생성물 1

HCID 49820158HCID 49820158, 화합물

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

To a solution of compound 9 (100 mg, 0.371 mmol) in DMSO (1.5 mL) was added Dess-Martin periodinane (315 mg, 0.743 mmol) at 0° C. The resulting mixture was stirred at room temperature for 20 min and poured into ice water (2 mL). The resulting precipitate was filtered, washed with water, and dried under high vacuum to obtain compound SKC-BF-02 (50 mg, 50%) as a red solid. Rf=0.6 (CHCl3-MeOH, 9:1); 1H NMR (CDCl3) δ 7.85 (d, J=9.0 Hz, 2H), 7.81 (s, 1H), 7.40 (d, J=10.3 Hz, 1H), 6.93 (d, J=9.0 Hz, 2H), 6.32 (d, J=10.3 Hz, 1H), 3.88 (s, 3H); MS (ES) m/z 317 (M+H)+.

후처리

  1. filtrationThe resulting precipitate was filtered
  2. washwashed with water
  3. customdried under high vacuum
  4. customto obtain compound SKC-BF-02 (50 mg, 50%) as a red solid

출처 및 근거

ORD 기록
ord-19b99308c98c45dfb531f55ffbeb10ee
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08614237B2

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