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Phosphorus pentachloride → HCID 67436031, 화합물

HRID 82734
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HRID 82734 반응식
[C:1]([C:3]1[CH:4]=[C:5]([CH:29]=[CH:30][CH:31]=1)[C:6]([NH:8][C:9]1[C:13]([C:14]2[N:18]([C:19]3[CH:24]=[CH:23][C:22]([F:25])=[C:21]([C:26]#[N:27])[CH:20]=3)[C:17](=[O:28])[O:16][N:15]=2)=[N:12][O:11][N:10]=1)=O)#[N:2].P(Cl)(Cl)(Cl)(Cl)Cl.C([BH3-])#N.[Na+]>C1C=CC=CC=1>[C:1]([C:3]1[CH:4]=[C:5]([CH:29]=[CH:30][CH:31]=1)[CH2:6][NH:8][C:9]1[C:13]([C:14]2[N:18]([C:19]3[CH:24]=[CH:23][C:22]([F:25])=[C:21]([CH:20]=3)[C:26]#[N:27])[C:17](=[O:28])[O:16][N:15]=2)=[N:12][O:11][N:10]=1)#[N:2]
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참가 물질

5

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HCID 24819Phosphorus pentachlorideHCID 5003444Sodium cyanoborohydrideHCID 674356943-cyano-N-{4-[4-(3-cyano-4-fluorophenyl)-5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl]-1,2,5-oxadiazol-3-yl}benzamide

생성물 1

HCID 67436031HCID 67436031, 화합물

시약·촉매·용매 1

HCID 241Benzene용매

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온도
90 °C

실험 절차

A solution of 3-cyano-N-{4-[4-(3-cyano-4-fluorophenyl)-5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl]-1,2,5-oxadiazol-3-yl}benzamide (30 mg, 72 μmol) in benzene (2 mL) at 0° C. was treated with phosphorus pentachloride (45 mg, 0.22 mmol) and stirred at 90° C. for 2 h. The reaction mixture was concentrated, diluted with ethanol (2.5 mL), treated with sodium cyanoborohydride (14 mg, 0.22 mmol), and stirred for 16 h. The reaction mixture was purified by preparative LCMS to give the intermediate 5-[3-{4-[(3-cyanobenzyl)amino]-1,2,5-oxadiazol-3-yl}-5-oxo-1,2,4-oxadiazol-4(5H)-yl]-2-fluorobenzonitrile. This material was diluted with ethanol (1 mL), treated with 2.0 M sodium hydroxide in water (0.2 mL), and stirred for 45 min. Purification of the crude reaction mixture by preparative HPLC gave the desired product (3 mg, 11%). LCMS for C18H13FN7O2 (M+H)+: m/z=378.0.

후처리

  1. concentrationThe reaction mixture was concentrated
  2. additiondiluted with ethanol (2.5 mL)
  3. stirringstirred for 16 h
  4. customThe reaction mixture was purified by preparative LCMS

출처 및 근거

ORD 기록
ord-3a541b32effe448993e34552296777c4
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08846726B2

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