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Tetrahydrofuran → HCID 59560500, 화합물

HRID 1176179
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HRID 1176179 반응식
C[Si]([C:5]#[C:6][C:7]1[C:15]2[C:11](=[N:12][S:13][N:14]=2)[CH:10]=[CH:9][CH:8]=1)(C)C.C([O-])([O-])=O.[K+].[K+].C1COCC1>CO>[C:6]([C:7]1[C:15]2[C:11](=[N:12][S:13][N:14]=2)[CH:10]=[CH:9][CH:8]=1)#[CH:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 11430Potassium CarbonateHCID 68407726HCID 68407726, 화합물

생성물 1

HCID 59560500HCID 59560500, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

4-(Trimethylsilyl)ethynylbenzo[c][1,2,5]-thiadiazole (0.100 g, 4.30×10−4 mol), K2CO3 (78.6 mg, 5.71×10−4 mol), THF (3 ml), and MeOH (2 ml) were added to a 25-ml Schlenk tube. The mixture was purged with N2 for 5 min, following which the reaction was stirred at room temperature for 1.5 h. The reaction mixture was then filtered, evaporated, and chromatographed on silica gel using 5:1 hexanes:THF as the eluent. Yield=63 g (91.4% based on 0.100 g of 4-(trimethylsilyl)ethynylbenzothiadiazole). 1H NMR (500 MHz, CDCl3): δ 8.01 (m, 1H, Ph-H), 7.78 (m, 1H, Ph-H), 7.56 (m, 1H, Ph-H), 3.56 (s, 1H, —CC—H).

후처리

  1. customThe mixture was purged with N2 for 5 min
  2. filtrationThe reaction mixture was then filtered
  3. customevaporated
  4. customchromatographed on silica gel using 5:1 hexanes

출처 및 근거

ORD 기록
ord-998aafdc00d244c798f7d46b5ac91a75
출처 데이터셋
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07842758B2

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