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HCID 10314079, 화합물 → HCID 136351968, 화합물

HRID 601303
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HRID 601303 반응식
[NH2:1][C:2]1[S:3][CH:4]=[C:5]([CH2:11][O:12][CH2:13][O:14][CH3:15])[C:6]=1[S:7]([NH2:10])(=[O:9])=[O:8].CS[C:18](SC)=[C:19]1[C:28](=[O:29])[C:27]2[C:22](=[N:23][CH:24]=[CH:25][CH:26]=2)[N:21]([CH2:30][CH2:31][CH2:32][CH3:33])[C:20]1=[O:34]>C1(C)C=CC=CC=1>[CH2:30]([N:21]1[C:22]2[C:27](=[CH:26][CH:25]=[CH:24][N:23]=2)[C:28]([OH:29])=[C:19]([C:18]2[NH:1][C:2]3[S:3][CH:4]=[C:5]([CH2:11][O:12][CH2:13][O:14][CH3:15])[C:6]=3[S:7](=[O:8])(=[O:9])[N:10]=2)[C:20]1=[O:34])[CH2:31][CH2:32][CH3:33]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 10314079HCID 10314079, 화합물HCID 574551872-Amino-4-[(methoxymethoxy)methyl]-3-thiophenesulfonamide

생성물 1

HCID 136351968HCID 136351968, 화합물수율 55.4%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

The product of Example 309G (110 mg, 0.43 mmol) and the product of Example 315B (140.6 mg, 0.43 mmol) were reacted in toluene (5 mL) at 100° C. for 3 hours. The reaction was concentrated under reduced pressure and the residue was purified by chromatography on silica gel using a Biotage-12 m column eluting with 1:99 methanol:dichloromethane to give the title compound as a white solid (114 mg, 54.6%). The sodium salt of the title compound was prepared according to the procedure of Example 1D. 1H NMR (300 MHz,CDCCl3) δ ppm 1.00 (t, J=7.35 Hz, 3 H), 1.46 (m, 2 H), 1.74 (m, 2 H), 3.45 (s, 3 H), 4.56 (m, 2 H), 4.80 (s, 2 H), 4.84 (s, 2 H), 7.09 (s, 1 H), 7.26 (s, 1 H), 7.36 (dd, J=8.09, 4.41 Hz, 1 H), 8.57 (dd, J=8.09, 1.84 Hz, 1 H), 8.81 (dd, J=4.78, 1.84 Hz, 1 H), 15.06 (s, 1 H), 15.11 (s, 1 H).

후처리

  1. concentrationThe reaction was concentrated under reduced pressure
  2. customthe residue was purified by chromatography on silica gel using a Biotage-12 m column
  3. washeluting with 1:99 methanol

출처 및 근거

ORD 기록
ord-4464ead5c7954194a94e10f6ebb47d29
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07902203B2

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