Water → 4-[6-(2,2-Difluoroethoxy)-2,4-dioxo-3,4-dihydroquinazolin-1(2H)-yl]piperidine-1-carbaldehyde

HRID 80476노트

반응식

HRID 80476 반응식
[F:1][CH:2]([F:23])[CH2:3][O:4][C:5]1[CH:6]=[C:7]2[C:12](=[CH:13][CH:14]=1)[N:11]([CH:15]1[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]1)[C:10](=[O:21])[NH:9][C:8]2=[O:22].[CH:24]([O-])=[O:25].[NH4+].O>C(#N)C.O1CCOCC1>[F:23][CH:2]([F:1])[CH2:3][O:4][C:5]1[CH:6]=[C:7]2[C:12](=[CH:13][CH:14]=1)[N:11]([CH:15]1[CH2:16][CH2:17][N:18]([CH:24]=[O:25])[CH2:19][CH2:20]1)[C:10](=[O:21])[NH:9][C:8]2=[O:22]

참가 물질

6

반응물 3

HCID 962WaterHCID 2723923Ammonium formateHCID 866478036-(2,2-Difluoroethoxy)-1-(piperidin-4-yl)quinazoline-2,4(1H,3H)-dione

생성물 1

HCID 252533494-[6-(2,2-Difluoroethoxy)-2,4-dioxo-3,4-dihydroquinazolin-1(2H)-yl]piperidine-1-carbaldehyde수율 67.1%

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 312751,4-Dioxane용매

실험 절차

A mixture of 6.13 g of 6-(2,2-difluoroethoxy)-1-(piperidin-4-yl) quinazoline-2,4(1H,3H)-dione obtained in stage 3.6 and 3.12 g of ammonium formate in 28 ml of ACN and 28 ml of dioxane is irradiated under a microwave field at 140° C. for 1 h 00. The reaction mixture is run into water. The mixture is filtered and the precipitate is washed with water and then with ether to give 4.47 g of the expected product.

후처리

  1. customis irradiated under a microwave field at 140° C. for 1 h 00
  2. filtrationThe mixture is filtered
  3. washthe precipitate is washed with water

출처 및 근거

ORD 기록
ord-9b39af9311df43a78db2157a8f8d895d
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846654B2

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