Dichloromethane → HCID 59397874、化合物

HRID 2193230ノート

反応式

HRID 2193230 の反応式
ClCCl.[C:4]([O:8][C:9]([N:11]([CH2:35][C:36]1[CH:45]=[CH:44]C2OCCOC=2[CH:37]=1)[CH:12]1[CH2:17][CH2:16][N:15]([CH2:18][CH2:19][N:20]2[C:29]3[C:24](=[CH:25][CH:26]=[C:27]([C:30](O)=[O:31])[CH:28]=3)[C:23]([CH3:33])=[CH:22][C:21]2=[O:34])[CH2:14][CH2:13]1)=[O:10])([CH3:7])([CH3:6])[CH3:5].Cl.[CH3:47][NH:48][CH3:49].F[P-](F)(F)(F)(F)F.N1([O:66][C:67](N(C)C)=[N+](C)C)C2N=CC=CC=2N=N1.[C:74]([O:77][CH2:78]C)(=O)[CH3:75]>O.C(N(CC)CC)C>[O:66]1[C:67]2[CH:44]=[CH:45][C:36]([CH2:35][N:11]([CH:12]3[CH2:13][CH2:14][N:15]([CH2:18][CH2:19][N:20]4[C:29]5[C:24](=[CH:25][CH:26]=[C:27]([C:30]([N:48]([CH3:49])[CH3:47])=[O:31])[CH:28]=5)[C:23]([CH3:33])=[CH:22][C:21]4=[O:34])[CH2:16][CH2:17]3)[C:9](=[O:10])[O:8][C:4]([CH3:7])([CH3:6])[CH3:5])=[CH:37][C:78]=2[O:77][CH2:74][CH2:75]1

参加物

8

反応物 5

HCID 6344DichloromethaneHCID 8857Ethyl AcetateHCID 10473Dimethylamine, hydrochlorideHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 59397939HCID 59397939、化合物

生成物 1

HCID 59397874HCID 59397874、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8471Triethylamine溶媒

実験手順

To 1.7 mL of a dichloromethane solution containing 0.10 g of 1-(2-(4-((tert-butoxycarbonyl)(2,3-dihydro-1,4-benzodioxin-6-ylmethyl)amino)piperidin-1-yl)ethyl)-4-methyl-2-oxo-1,2-dihydroquinoline-7-carboxylic acid, 89 μL of triethylamine, 51 mg of dimethylamine hydrochloride and 0.12 g of O-(7-azabenzotriazol-1-yl)-1,1,3,3-tetramethyluronium hexafluorophosphate were added at room temperature, and stirred at the same temperature for 1 hour. Water and ethyl acetate were added to the reaction mixture. The organic layer was separated, washed with aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. The residue thus obtained was purified by basic silica gel column chromatography [eluent; chloroform:methanol=100:1], to give 93 mg of tert-butyl (2,3-dihydro-1,4-benzodioxin-6-ylmethyl)(1-(2-(7-((dimethylamino)carbonyl)-4-methyl-2-oxoquinolin-1(2H)-yl)ethyl)piperidin-4-yl)carbamate as a white solid.

後処理

  1. additionwere added at room temperature
  2. customThe organic layer was separated
  3. washwashed with aqueous saturated sodium chloride solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customthe solvent was removed under reduced pressure
  6. customThe residue thus obtained
  7. customwas purified by basic silica gel column chromatography [eluent; chloroform:methanol=100:1]

出典と根拠

ORDレコード
ord-55b7cd95f1fc4b9c9d7922ca85d89e78
出典データセット
uspto-grants-2012_12
特許番号
US08329694B2

反応ノート

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