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Acetonitrile → HCID 19858044, 화합물

HRID 2073391
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HRID 2073391 반응식
Cl[CH:2]([C:10]1[CH:22]=[C:21]2[C:13]([CH:14]=[CH:15][C:16]3[O:17][C:18](=[O:25])[C:19](C)(C)[C:20]=32)=[CH:12][CH:11]=1)[C:3]1[CH:8]=[CH:7][C:6]([Cl:9])=[CH:5][CH:4]=1.[NH:26]1[CH:30]=[N:29][CH:28]=[N:27]1.C(=O)([O-])[O-].[K+].[K+].C(#N)C>O>[Cl:9][C:6]1[CH:7]=[CH:8][C:3]([CH:2]([C:10]2[CH:22]=[C:21]3[C:13]([CH:14]=[CH:15][C:16]4[O:17][C:18](=[O:25])[CH2:19][C:20]=43)=[CH:12][CH:11]=2)[N:26]2[CH:30]=[N:29][CH:28]=[N:27]2)=[CH:4][CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6342AcetonitrileHCID 92571H-1,2,4-TriazoleHCID 11430Potassium CarbonateHCID 19858036HCID 19858036, 화합물

생성물 1

HCID 19858044HCID 19858044, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 8-(α,4-dichlorobenzyl)-1,1-dimethyl-2(1H)-naphtho[2,1-b]furanone, 1,2,4-triazole (0.3 g), potassium carbonate (0.3 g) and acetonitrile (5 ml) was heated under reflux for 18 h. The mixture was treated with water (20 ml) and extracted with ethyl acetate. The ethyl acetate extract was dried and then evaporated to dryness, and the residue was purified by flash chromatography eluting with methanol:chloroform, 1:99 v/v, to give 8-[4-chloro-α-(1H-1,2,4-triazol-1-yl)benzyl]-2(1H)-naphtho[2,1-b]furanone. Nmr in deuteriochloroform: δ8.12(2H,s); 7.94(1H,d); 7.36-7.46(4H,m); 7.15-7.25(3H,m); 6.92(1H,s); 1.62(3H,s); 1.60(3H,s).

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 18 h
  3. extractionextracted with ethyl acetate
  4. extractionThe ethyl acetate extract
  5. customwas dried
  6. customevaporated to dryness
  7. customthe residue was purified by flash chromatography
  8. washeluting with methanol

출처 및 근거

ORD 기록
ord-093a5c9bfbd44dc2b50e184e2ece372a
출처 데이터셋
uspto-grants-1990_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04916148

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