Ethanolamine → HCID 59398197、化合物

HRID 2193190

反応式

HRID 2193190 の反応式
[C:1]([O:5][C:6]([N:8]([CH2:33][C:34]1[CH:43]=[CH:42][C:37]2[O:38][CH2:39][CH2:40][O:41][C:36]=2[CH:35]=1)[CH:9]1[CH2:14][CH2:13][N:12]([CH2:15][CH2:16][N:17]2[C:26]3[C:21](=[CH:22][CH:23]=[C:24]([O:27][CH3:28])[CH:25]=3)[C:20]([C:29](O)=[O:30])=[CH:19][C:18]2=[O:32])[CH2:11][CH2:10]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C(Cl)(=O)OCC.[NH2:50][CH2:51][CH2:52][OH:53].C(OC(C)C)(C)C>C(OCC)C.O.C(OCC)(=O)C.C(N(CC)CC)C.O1CCCC1>[C:1]([O:5][C:6](=[O:7])[N:8]([CH2:33][C:34]1[CH:43]=[CH:42][C:37]2[O:38][CH2:39][CH2:40][O:41][C:36]=2[CH:35]=1)[CH:9]1[CH2:14][CH2:13][N:12]([CH2:15][CH2:16][N:17]2[C:26]3[C:21](=[CH:22][CH:23]=[C:24]([O:27][CH3:28])[CH:25]=3)[C:20]([C:29]([NH:50][CH2:51][CH2:52][OH:53])=[O:30])=[CH:19][C:18]2=[O:32])[CH2:11][CH2:10]1)([CH3:4])([CH3:2])[CH3:3]

参加物

10

反応物 4

HCID 700Ethanolamine3 回HCID 7914Diisopropyl EtherHCID 10928Ethyl chloroformateHCID 593981451-(2-(4-((Tert-butoxycarbonyl)(2,3-dihydro-1,4-benzodioxin-6-ylmethyl)amino)piperidin-1-yl)ethyl)-7-methoxy-2-oxo-1,2-dihydroquinoline-4-carboxylic acid

生成物 1

HCID 59398197HCID 59398197、化合物

試薬・触媒・溶媒 5

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒HCID 8471Triethylamine溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To 3.0 mL of tetrahydrofuran suspension containing 0.15 g of 1-(2-(4-((tert-butoxycarbonyl)(2,3-dihydro-1,4-benzodioxin-6-ylmethyl)amino)piperidin-1-yl)ethyl)-7-methoxy-2-oxo-1,2-dihydroquinoline-4-carboxylic acid, 39 μL, of triethylamine was added at room temperature, 25 μL of ethyl chlorocarbonate was added dropwise under ice-cooling, and the reaction mixture was stirred at the same temperature for 2 hours. Then, 15 μL of 2-aminoethanol was added dropwise. After stirred at the same temperature for 3 hours, 15 μL of 2-aminoethanol was added dropwise and stirred for 1.5 hours. Further, 15 μL of 2-aminoethanol was added dropwise and stirred at room temperature for 40 min. To the reaction mixture, ethyl acetate and water were added, the organic layer was separated, and the aqueous layer was extracted with ethyl acetate. The organic layer and extracts were combined, washed sequentially with water and aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. To the residue thus obtained, diethyl ether and diisopropyl ether were added, and the resulting solid was filtered to give 84 mg of tert-butyl(2,3-dihydro-1,4-benzodioxin-6-ylmethyl)(1-(2-(4-(((2-hydroxyethyl)amino)carbonyl)-7-methoxy-2-oxoquinolin-1(2H)-yl)ethyl)piperidin-4-yl)carbamate as a slight yellow solid.

後処理

  1. temperaturecooling
  2. stirringAfter stirred at the same temperature for 3 hours
  3. stirringstirred for 1.5 hours
  4. stirringstirred at room temperature for 40 min
  5. customthe organic layer was separated
  6. extractionthe aqueous layer was extracted with ethyl acetate
  7. washwashed sequentially with water and aqueous saturated sodium chloride solution
  8. dry with materialdried over anhydrous magnesium sulfate
  9. customthe solvent was removed under reduced pressure
  10. customTo the residue thus obtained
  11. filtrationthe resulting solid was filtered

出典と根拠

ORDレコード
ord-24052c1446f54e8bb42180f4a03daf85
出典データセット
uspto-grants-2012_12
特許番号
US08329694B2

関連ノート

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