Dichloromethane → HCID 86759736、化合物

HRID 2182551ノート

反応式

HRID 2182551 の反応式
C1CCN([C:7](/N=N/C(N2CCCCC2)=O)=[O:8])CC1.O[C:20]1[CH:29]=[C:28]2[C:23]([CH:24]=[N:25][C:26](OC)=[N:27]2)=[CH:22][CH:21]=1.C1(OCCO)CCCC1.C(P(CCCC)CCCC)CCC.C(Cl)[Cl:55]>CCOCC>[ClH:55].[CH3:7][O:8][C:24]1[C:23]2[C:28](=[CH:29][CH:20]=[CH:21][CH:22]=2)[N:27]=[CH:26][N:25]=1

参加物

7

反応物 5

HCID 6344DichloromethaneHCID 13831TributylphosphineHCID 5702657diazenedicarboxylic acid bis(N,N-piperidide)HCID 131875202-(Cyclopentyloxy)ethan-1-olHCID 136399837HCID 136399837、化合物

生成物 1

HCID 86759736HCID 86759736、化合物収率 60%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

1,1-(Azodicarbonyl)dipiperidine (355 mg, 1.4 mmol) was added in portions to a mixture of 44-chloro-2-fluoroanilino)-7-hydroxy-methoxyquinazoline (I 50 mg, 0.47 mmol), (prepared as described for the starting material in Example 2), 2-(cyclopentyloxy)ethanol (91 mg, 0.7 mmol), (U.S. Pat. No. 4,515,814), and tributylphosphine (284 mg, 1.4 mmol) in methylene chloride (6 ml) at 0° C. The mixture was then allowed to warm to ambient temperature and stirred for 3.5 hours. Ether (3 ml) was added and the insolubles were removed by filtration and the volatiles were removed from the filtrate by evaporation. The residue was dissolved in acetone and 1M ethereal hydrogen chloride (0.6 ml) was added. The mixture was left to stand for 60 hours and the precipitate was collected by filtration, washed with acetone and dried to give 44-chloro-2-fluoroanilino)-72-cyclopentyl xyethoxy)-4-methoxyquinazoline hydrochloride (130 mg, 60%).

後処理

  1. custom(prepared
  2. customat 0° C
  3. customthe insolubles were removed by filtration
  4. customthe volatiles were removed from the filtrate by evaporation
  5. dissolutionThe residue was dissolved in acetone
  6. addition1M ethereal hydrogen chloride (0.6 ml) was added
  7. waitThe mixture was left
  8. waitto stand for 60 hours
  9. filtrationthe precipitate was collected by filtration
  10. washwashed with acetone
  11. customdried

出典と根拠

ORDレコード
ord-f468ebb7b5a242c2ae43886d535a358b
出典データセット
uspto-grants-2005_05
特許番号
US06897210B2

反応ノート

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