Hydrochloric Acid → HCID 22181238, 화합물

HRID 1796190노트

반응식

HRID 1796190 반응식
[C:1]([C:4]1[CH:5]=[C:6](/[CH:10]=[CH:11]/[CH2:12][N:13]([C:18]2[CH:23]=[CH:22][C:21]([O:24][CH:25]3[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]3)=[C:20]([C:31](=[O:33])[NH2:32])[CH:19]=2)[S:14]([CH3:17])(=[O:16])=[O:15])[CH:7]=[CH:8][CH:9]=1)(=[NH:3])[NH2:2].C(O[C:37]1[O:38][CH2:39][CH2:40][N:41]=1)C.O1CC(=O)N=[C-]1.C(N(CC)CC)C.[ClH:55]>CO>[ClH:55].[ClH:55].[C:1]([C:4]1[CH:5]=[C:6](/[CH:10]=[CH:11]/[CH2:12][N:13]([C:18]2[CH:23]=[CH:22][C:21]([O:24][CH:25]3[CH2:30][CH2:29][N:28]([C:37]4[O:38][CH2:39][CH2:40][N:41]=4)[CH2:27][CH2:26]3)=[C:20]([C:31](=[O:33])[NH2:32])[CH:19]=2)[S:14]([CH3:17])(=[O:16])=[O:15])[CH:7]=[CH:8][CH:9]=1)(=[NH:2])[NH2:3]

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 127306402-Ethoxy-4,5-dihydro-1,3-oxazoleHCID 22180972N-[3-(3-amidinophenyl)-2-(E)-propenyl]-N-[3-carbamoyl-4-(piperidin-4-yloxy)phenyl]methanesulfonamideHCID 532495662H-1,3-oxazol-2-id-4-one

생성물 1

HCID 22181238HCID 22181238, 화합물수율 59%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of N-[3-(3-amidinophenyl)-2-(E)-propenyl]-N-[3-carbamoyl-4-(piperidin-4-yloxy)phenyl]methanesulfonamide (0.32 g) obtained in example 99(a) in methanol (15 ml) were added successively 2-ethoxy-4,5-dihydrooxazole (0.21 g), which was prepared from 2-oxazolidone according to the method described in Eur. J. Org. Chem., 10, 2645 (1999), and triethylamine (0.56 ml) at room temperature, and the resulting mixture was stirred at room temperature for 2 hours and allowed to stand at room temperature overnight and then evaporated in vacuo. The residue obtained was purified by preparative HPLC (YMC-Pack ODS-A; YMC, eluent: 12% acetonitrile/water). The amorphous solid obtained was dissolved in 1N hydrochloric acid (1.2 ml) and evaporated to dryness in vacuo to afford the title compound (0.15 g, yield: 59%) as a colorless amorphous solid.

후처리

  1. customevaporated in vacuo
  2. customThe residue obtained
  3. customwas purified by preparative HPLC (YMC-Pack ODS-A; YMC, eluent: 12% acetonitrile/water)
  4. customThe amorphous solid obtained
  5. customevaporated to dryness in vacuo

출처 및 근거

ORD 기록
ord-2a708e91a13a43d19cf8554f0b6df25b
출처 데이터셋
uspto-grants-2006_04
특허 번호
US07030138B2

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