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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Allyl bromide → HCID 19737997, 화합물

HRID 2255506
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HRID 2255506 반응식
[OH:1][CH:2]1[C:7]2[CH:8]=[CH:9][S:10][C:6]=2[S:5](=[O:12])(=[O:11])[NH:4][CH2:3]1.[H-].[Na+].[CH2:15](Br)[CH:16]=[CH2:17]>CN(C=O)C>[CH2:17]([N:4]1[CH2:3][CH:2]([OH:1])[C:7]2[CH:8]=[CH:9][S:10][C:6]=2[S:5]1(=[O:12])=[O:11])[CH:16]=[CH2:15]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7841Allyl bromideHCID 24758Sodium hydrideHCID 229019424-Hydroxy-3,4-dihydro-2H-thieno[3,2-e][1,2]thiazine 1,1-dioxide

생성물 1

HCID 19737997HCID 19737997, 화합물수율 88%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
-10 °C

실험 절차

The product from Step C of Example 2 (4.0 g, 19.5 mmol) was dissolved in anhydrous DMF (70 mL) cooled to -10° C. and sodium hydride (21.5 mmol) was added. After stirring for five minutes allyl bromide (2.53 mL, 29.25 mmol) was added and this mixture stirred for 2 h at 0° C. The reaction mixture was poured onto ice water (100 mL) and this solution was extracted with ethyl acetate. The combined extracts were washed with brine, dried (MgSO4) and evaporated to give a crude product which was purified by column chromatography (silica, methylene chloride:methanol, 20:1) to provide the desired product (4.2 g, 88%) as a syrup.

후처리

  1. additionwas added
  2. additionThe reaction mixture was poured onto ice water (100 mL)
  3. extractionthis solution was extracted with ethyl acetate
  4. washThe combined extracts were washed with brine
  5. dry with materialdried (MgSO4)
  6. customevaporated
  7. customto give a crude product which
  8. customwas purified by column chromatography (silica, methylene chloride:methanol, 20:1)

출처 및 근거

ORD 기록
ord-787f612a7ee14d269243e2299d5df1d9
출처 데이터셋
uspto-grants-1993_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05240923

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