Dichloromethane → HCID 59397874, 화합물

HRID 39857노트

반응식

HRID 39857 반응식
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

참가 물질

8

반응물 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, 화합물

생성물 1

HCID 59397874HCID 59397874, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8471Triethylamine용매

실험 절차

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.

후처리

  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]

출처 및 근거

ORD 기록
ord-b32135c7894c424aa4f11c4c5bd11b21
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08524738B2

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