Acetic Anhydride → HCID 86690906, 화합물

HRID 72663

반응식

HRID 72663 반응식
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH2:12][S:13]([CH2:16][C:17](O)=O)(=[O:15])=[O:14])=[N:7][C:8]=1[N+:9]([O-:11])=[O:10].[CH3:20][O:21][C:22]1[CH:29]=[C:28]([O:30][CH3:31])[CH:27]=[C:26]([O:32][CH3:33])[C:23]=1C=O.C(OC(=O)C)(=O)C>C1(C)C=CC=CC=1>[CH3:1][O:2][C:3]1[C:8]([N+:9]([O-:11])=[O:10])=[N:7][C:6]([CH2:12][S:13](/[CH:16]=[CH:17]/[C:23]2[C:26]([O:32][CH3:33])=[CH:27][C:28]([O:30][CH3:31])=[CH:29][C:22]=2[O:21][CH3:20])(=[O:14])=[O:15])=[CH:5][CH:4]=1

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 700192,4,6-TrimethoxybenzaldehydeHCID 67994551HCID 67994551, 화합물

생성물 1

HCID 86690906HCID 86690906, 화합물수율 35.3%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of 2-((5-methoxy-6-nitropyridin-2-yl)methylsulfonyl)acetic acid (0.29 g, 1.0 mmol) in dry toluene (2 mL) was added 2,4,6-trimethoxybenz-aldehyde (0.196 g, 1.0 mmol) and acetic anhydride (0.38 mL). After refluxing for 5 hrs, the reaction mixture was evaporated to dryness. The residue was precipitated by adding methanol (15 mL). The precipitate was filtered to give 150 mg (35%) the titled compound as grey coloured powder. 1H-NMR (Acetone-D6): δ 3.92 (s, 9H, 3×OCH3), 4.07 (s, 3H, OCH3), 4.52 (s, 2H, CH2), 6.32 (s, 2H, Ph-H), 7.20 (d, J=15.6 Hz, 1H, CH), 7.74 (d, 1H, J=15.6 Hz, CH), 7.87 (d, 1H, J=8.4 Hz, Py-H), 7.95 (d, 1H, J=8.8 Hz, Py-H); HR-MS (ESI+) m/z 425.1053 [M+1]+ C18H20N2O8S requires 424.0940.

후처리

  1. temperatureAfter refluxing for 5 hrs
  2. customthe reaction mixture was evaporated to dryness
  3. customThe residue was precipitated
  4. additionby adding methanol (15 mL)
  5. filtrationThe precipitate was filtered

출처 및 근거

ORD 기록
ord-e8c7e36a8cd9498bb2743f95ead1cd29
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08829003B2

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