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Methyl iodide → HCID 135741846, 화합물

HRID 732932
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HRID 732932 반응식
[OH:1][CH:2]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[CH2:3][N:4]1[C:8]2[NH:9][C:10](=[S:14])[NH:11][C:12](=[O:13])[C:7]=2[CH:6]=[N:5]1.[CH3:21]I>C1COCC1>[OH:1][CH:2]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[CH2:3][N:4]1[C:8]2[N:9]=[C:10]([S:14][CH3:21])[NH:11][C:12](=[O:13])[C:7]=2[CH:6]=[N:5]1
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참가 물질

4

반응물 2

HCID 6328Methyl iodideHCID 136383527HCID 136383527, 화합물

생성물 1

HCID 135741846HCID 135741846, 화합물수율 72%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 7 (2.88 g, 10 mmol) and methyl iodide (7.10 g, 50 mmol) in anhydrous THF (20 mL) was refluxed for 12 h. The solvent and the excess of methyl iodide were removed by distillation under reduced pressure; the oil residue crystallized by adding CHCl3 (10 mL) and was purified by recrystallization with absolute ethanol to give 8a (2.17 g, 72%) as a white solid; mp 208-209° C. 1H NMR: δ 2.51 (s, 3H, CH3), 4.27-4.50 (m, 2H, CH2N), 5.04-5.18 (m, 1H, CHO), 5.68 (d, 1H, OH, disappears with D2O), 7.20-7.42 (m, 5H Ar), 7.97 (s, 1H, H-3). IR cm−1: 3544 (NH), 3450-3350 (OH), 1678 (CO). Anal. (C14H14N4O2S) C, H, N, S.

후처리

  1. customThe solvent and the excess of methyl iodide were removed by distillation under reduced pressure
  2. customthe oil residue crystallized
  3. additionby adding CHCl3 (10 mL)
  4. customwas purified by recrystallization with absolute ethanol

출처 및 근거

ORD 기록
ord-42cbe7e89d574d32a49ff7bc652e5f7f
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07589086B2

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