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Acetic Acid → HCID 136383527, 화합물

HRID 732931
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HRID 732931 반응식
C([NH:9][C:10]([NH:12][C:13]1[N:17]([CH2:18][CH:19]([OH:26])[C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[N:16]=[CH:15][C:14]=1[C:27]([O:29]CC)=O)=[S:11])(=O)C1C=CC=CC=1.C(O)(=O)C>[OH-].[Na+].O>[OH:26][CH:19]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[CH2:18][N:17]1[C:13]2[NH:12][C:10](=[S:11])[NH:9][C:27](=[O:29])[C:14]=2[CH:15]=[N:16]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 176Acetic AcidHCID 86609906HCID 86609906, 화합물

생성물 1

HCID 136383527HCID 136383527, 화합물수율 80%

시약·촉매·용매 2

HCID 962Water용매HCID 14798Sodium Hydroxide용매

실험 절차

A solution of 6 (4.38 g, 10 mmol) in 2 M NaOH (40 mL) was refluxed for 10 min and successively diluted with H2O (40 mL). The solution was acidified with glacial acetic acid. Standing in a refrigerator for 12 h, a solid crystallized, and was filtered and recrystallized from absolute ethanol to give 7 (2.3 g, 80%) as a white solid; mp 264-265° C. 1H NMR: δ 4.15-4.30 and 4.55-4.72 (2m, 2H, CH2N), 4.85-5.00 (m, 1H, CHO), 5.66 (br s, 1H, OH, disappears with D2O), 7.20-7.51 (m, 5H Ar), 8.02 (s, 1H, H-3), 12.20 (s, 1H, NH, disappears with D2O), 13.40 (s, 1H, NH, disappears with D2O). IR cm−1: 3362 (NH), 3142-2773 (OH), 1681 (CO). Anal. (C13H12N4O2S) C, H, N, S.

후처리

  1. customa solid crystallized
  2. filtrationwas filtered
  3. customrecrystallized from absolute ethanol

출처 및 근거

ORD 기록
ord-7c2de85b7bf1413ab5a66d9f2c8636c8
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07589086B2

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