Hydrochloric Acid → HCID 22181238、化合物

HRID 1796190ノート

反応式

HRID 1796190 の反応式
[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]

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 127306402-Ethoxy-4,5-dihydro-1,3-oxazoleHCID 22180972HCID 22180972、化合物HCID 532495662H-1,3-oxazol-2-id-4-one

生成物 1

HCID 22181238HCID 22181238、化合物収率 59%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2a708e91a13a43d19cf8554f0b6df25b
出典データセット
uspto-grants-2006_04
特許番号
US07030138B2

反応ノート

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