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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Iodoethane → HCID 87546601, 화합물

HRID 1435691
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HRID 1435691 반응식
[H-].[Na+].[Cl:3][C:4]1[C:5]([CH3:22])=[C:6]([S:10]([NH:13][C:14]2[S:15][CH:16]=[C:17]([CH2:19][CH2:20][OH:21])[N:18]=2)(=[O:12])=[O:11])[CH:7]=[CH:8][CH:9]=1.[CH2:23](I)[CH3:24]>O1CCCC1>[Cl:3][C:4]1[C:5]([CH3:22])=[C:6]([S:10]([NH:13][C:14]2[S:15][CH:16]=[C:17]([CH2:19][CH2:20][O:21][CH2:23][CH3:24])[N:18]=2)(=[O:11])=[O:12])[CH:7]=[CH:8][CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6340IodoethaneHCID 24758Sodium hydrideHCID 87545745HCID 87545745, 화합물

생성물 1

HCID 87546601HCID 87546601, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Sodium hydride (95% dry, 80 mg, 3.23 mmol) was added to a stirred solution of EXAMPLE 181A (426 mg, 1.28 mmol) in tetrahydrofuran (10 mL) at room temperature. After stirring for 15 min, the mixture was treated with ethyl iodide (400 mg, 2.56 mmol). The reaction mixture was stirred for 2 h at 55° C. and then quenched with aqueous HCl (1 M, 1 mL) and water was added. The product was extracted with DCM and dried (Sodium sulfate). Evaporation of the solvent gave a residue which was purified by flash chromatography on silica gel eluting with 10% acetone in DCM giving an oil (0.25 g, 54%) which solidified on standing: MS (Ionspray, [M+H]+) m/z 360; Anal. Calcd. (found) for C14H17ClN2O3S2: C, 46.6 (46.5)%; H, 4.7 (4.6)%; N, 7.8 (7.8)%.

후처리

  1. stirringThe reaction mixture was stirred for 2 h at 55° C.
  2. customquenched with aqueous HCl (1 M, 1 mL) and water
  3. additionwas added
  4. extractionThe product was extracted with DCM
  5. dry with materialdried (Sodium sulfate)
  6. customEvaporation of the solvent
  7. customgave a residue which
  8. customwas purified by flash chromatography on silica gel eluting with 10% acetone in DCM giving an oil (0.25 g, 54%) which

출처 및 근거

ORD 기록
ord-71100907b9134f029d244bff2f8d63d0
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07618961B2

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