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Tetrahydrofuran → HCID 66914783, 화합물

HRID 2173039
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HRID 2173039 반응식
[H-].[Na+].C1COCC1.CC1C=CC(S(O[CH2:19][CH2:20][N:21]2[CH:25]=[C:24]([I:26])[CH:23]=[C:22]2[CH2:27][OH:28])(=O)=O)=CC=1>O>[I:26][C:24]1[CH:23]=[C:22]2[N:21]([CH:25]=1)[CH2:20][CH2:19][O:28][CH2:27]2
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참가 물질

5

반응물 3

HCID 8028Tetrahydrofuran2회HCID 24758Sodium hydrideHCID 86654671HCID 86654671, 화합물

생성물 1

HCID 66914783HCID 66914783, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a stirred mixture of sodium hydride (0.261 g, 6.53 mmol) and THF (10 mL) was slowly added a solution of 2-(2-(hydroxymethyl)-4-iodo-1H-pyrrol-1-yl)ethyl 4-methylbenzenesulfonate (2.75 g, 6.53 mmol) and THF (25 mL). The reaction mixture was stirred at room temperature for 30 hours, then diluted with water (20 mL) and extracted with EtOAc (2×60 mL). The organic phase was dried over sodium sulfate, evaporated, and purified using silica gel column (80 g) chromatography, eluting with a gradient of 0-100% hexane and EtOAc. The pure compound fractions were combined and evaporated to give the title compound as a tan solid, which turned green on standing (1.02 g, 63%). ESI-MS m/z [M+H]+ calc'd for C7H8INO, 250. found, 250.

후처리

  1. extractionextracted with EtOAc (2×60 mL)
  2. dry with materialThe organic phase was dried over sodium sulfate
  3. customevaporated
  4. custompurified
  5. washeluting with a gradient of 0-100% hexane and EtOAc
  6. customevaporated

출처 및 근거

ORD 기록
ord-2c7a64e12b4843528e16d7f398fc4399
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09056873B2

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