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Pyrrolidine → 1-Benzenesulfonyl-7-fluoro-3-(5-pyrrolidin-1-ylmethyl-thiophen-2-yl)-indole

HRID 644073
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HRID 644073 반응식
[C:1]1([S:7]([N:10]2[C:18]3[C:13](=[CH:14][CH:15]=[CH:16][C:17]=3[F:19])[C:12]([C:20]3[S:24][C:23]([CH:25]=O)=[CH:22][CH:21]=3)=[CH:11]2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[NH:27]1[CH2:31][CH2:30][CH2:29][CH2:28]1.C([BH3-])#N.[Na+]>C(O)(=O)C>[C:1]1([S:7]([N:10]2[C:18]3[C:13](=[CH:14][CH:15]=[CH:16][C:17]=3[F:19])[C:12]([C:20]3[S:24][C:23]([CH2:25][N:27]4[CH2:31][CH2:30][CH2:29][CH2:28]4)=[CH:22][CH:21]=3)=[CH:11]2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
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참가 물질

5

반응물 3

HCID 31268PyrrolidineHCID 5003444Sodium cyanoborohydrideHCID 860732925-(1-Benzenesulfonyl-7-fluoroindol-3-yl)-thiophene-2-carboxaldehyde

생성물 1

HCID 686951601-Benzenesulfonyl-7-fluoro-3-(5-pyrrolidin-1-ylmethyl-thiophen-2-yl)-indole

시약·촉매·용매 1

HCID 176Acetic Acid촉매

실험 절차

To the crude 5-(1-benzenesulfonyl-7-fluoroindol-3-yl)-thiophene-2-carboxaldehyde was sequentially added 4 Å molecular sieves (1 g), pyrrolidine (0.44 ml, 5.36 mmol), sodium cyanoborohydride (0.034 g, 0.54 mmol) and glacial acetic acid (1 drop). The resulting mixture was then stirred at room temperature for 18 h, filtered and the filter cake washed with methanol (2×30 ml) and dichloromethane (2×30 ml). The combined filtrate was concentrated in vacuo, dissolved in dichloromethane (20 ml), washed with aqueous sodium hydroxide (2M; 15 ml), dried with sodium sulphate and concentrated in vacuo. The residue was then purified by flash column chromatography eluting with 0-10% (v/v) methanol in dichloromethane to afford 1-benzenesulfonyl-7-fluoro-3-(5-pyrrolidin-1-ylmethyl-thiophen-2-yl)-indole as a yellow oil (0.22 g, 0.46 mmol).

후처리

  1. filtrationfiltered
  2. washthe filter cake washed with methanol (2×30 ml) and dichloromethane (2×30 ml)
  3. concentrationThe combined filtrate was concentrated in vacuo
  4. dissolutiondissolved in dichloromethane (20 ml)
  5. washwashed with aqueous sodium hydroxide (2M; 15 ml)
  6. dry with materialdried with sodium sulphate
  7. concentrationconcentrated in vacuo
  8. customThe residue was then purified by flash column chromatography
  9. washeluting with 0-10% (v/v) methanol in dichloromethane

출처 및 근거

ORD 기록
ord-108b4a2fa0f04bbfb94853844b5959f3
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07700634B2

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