Sodium Hydroxide → 1,1-Dimethylethyl 4-[6-(2,2-difluoroethoxy)-2,4-dioxo-3,4-dihydroquinazolin-1(2H)-yl]piperidine-1-carboxylate

HRID 403560

反応式

HRID 403560 の反応式
[C:1]([N:4]([C:18]1[CH:23]=[CH:22][C:21]([O:24][CH2:25][CH:26]([F:28])[F:27])=[CH:20][C:19]=1[C:29](OC)=[O:30])[CH:5]1[CH2:10][CH2:9][N:8]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:7][CH2:6]1)(=[O:3])[NH2:2].[OH-].[Na+]>O1CCOCC1>[F:27][CH:26]([F:28])[CH2:25][O:24][C:21]1[CH:20]=[C:19]2[C:18](=[CH:23][CH:22]=1)[N:4]([CH:5]1[CH2:6][CH2:7][N:8]([C:11]([O:13][C:14]([CH3:16])([CH3:17])[CH3:15])=[O:12])[CH2:9][CH2:10]1)[C:1](=[O:3])[NH:2][C:29]2=[O:30]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 595872271,1-Dimethylethyl 4-{carbamoyl[4-(2,2-difluoroethoxy)-2-(methoxycarbonyl)-phenyl]amino}piperidine-1-carboxylate

生成物 1

HCID 595871251,1-Dimethylethyl 4-[6-(2,2-difluoroethoxy)-2,4-dioxo-3,4-dihydroquinazolin-1(2H)-yl]piperidine-1-carboxylate

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

2.5 g of 1,1-dimethylethyl 4-{carbamoyl[4-(2,2-difluoroethoxy)-2-(methoxycarbonyl)phenyl]amino}piperidine-1-carboxylate obtained in stage 3.4 in solution in a mixture of 10 ml of dioxane and 5 ml of a 1N aqueous NaOH solution are irradiated under a microwave field at 130° C. for 30 min. Extraction is carried out with AcOEt and the extract is neutralized with a 1N aqueous HCl solution, washed with water, dried over MgSO4, filtered and evaporated under reduced pressure. The residue obtained is triturated in an AcOEt/pentane mixture to give the expected product. The same reaction is reproduced with 2 other lots of 2.5 g of 1,1-dimethylethyl 4-{carbamoyl[4-(2,2-difluoroethoxy)-2-(methoxycarbonyl)phenyl]amino}piperidine-1-carboxylate obtained in stage 3.4 to give, in total, 5.63 g of expected product.

後処理

  1. customare irradiated under a microwave field at 130° C. for 30 min
  2. extractionExtraction
  3. washwashed with water
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customevaporated under reduced pressure
  7. customThe residue obtained
  8. customis triturated in an AcOEt/pentane mixture

出典と根拠

ORDレコード
ord-0251afd642474ae793da05f61c4e1195
出典データセット
uspto-grants-2014_06
特許番号
US08748441B2

関連ノート

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