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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Sodium hydride → HCID 66914783, 화합물

HRID 880453
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HRID 880453 반응식
CC1C=CC(S(O[CH2:12][CH2:13][N:14]2[CH:18]=[C:17]([I:19])[CH:16]=[C:15]2[CH2:20][OH:21])(=O)=O)=CC=1.[H-].[Na+]>O1CCCC1>[I:19][C:17]1[CH:16]=[C:15]2[N:14]([CH:18]=1)[CH2:13][CH2:12][O:21][CH2:20]2
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참가 물질

4

반응물 2

HCID 24758Sodium hydrideHCID 86654671HCID 86654671, 화합물

생성물 1

HCID 66914783HCID 66914783, 화합물수율 67.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 2-[2-(hydroxymethyl)-4-iodo-pyrrol-1-yl]ethyl 4-methylbenzenesulfonate (2.0 g, 4.79 mmol) in tetrahydrofuran (15 mL) was slowly added to a suspension of sodium hydride (120 mg, 60% dispersion in mineral oil; 4.75 mmol) in tetrahydrofuran (5 mL) and stirred at room temperature for 36 h. The reaction was quenched with water and extracted with diethyl ether. The combined organic phases were washed with water, brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure to give a residue which was purified by column chromatography over silica gel using 2% ethyl acetate in petroleum ether to afford 7-iodo-3,4-dihydro-1H-pyrrolo[2,1-c][1,4]oxazine (800 mg, 66%) as a colorless crystalline solid.

후처리

  1. customThe reaction was quenched with water
  2. extractionextracted with diethyl ether
  3. washThe combined organic phases were washed with water, brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customto give a residue which
  7. customwas purified by column chromatography over silica gel using 2% ethyl acetate in petroleum ether

출처 및 근거

ORD 기록
ord-b9c482dfbfa34a629cb3a75f75e7309d
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08993574B2

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