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7-(2,4-Dimethoxybenzyl)-2-(ethylsulfanyl)-3-[4-(2,2,2-trifluoroethoxy)phenyl]-3,5,6,7-tetrahydropyrido[3,4-d]pyrimidine-4,8-dione → 2-(Ethylsulfanyl)-3-[4-(2,2,2-trifluoroethoxy)phenyl]-3,5,6,7-tetrahydropyrido[3,4-d]pyrimidine-4,8-dione

HRID 570729
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HRID 570729 반응식
COC1C=C(OC)C=CC=1C[N:6]1[CH2:15][CH2:14][C:13]2[C:12](=[O:16])[N:11]([C:17]3[CH:22]=[CH:21][C:20]([O:23][CH2:24][C:25]([F:28])([F:27])[F:26])=[CH:19][CH:18]=3)[C:10]([S:29][CH2:30][CH3:31])=[N:9][C:8]=2[C:7]1=[O:32]>C(O)=O>[CH2:30]([S:29][C:10]1[N:11]([C:17]2[CH:22]=[CH:21][C:20]([O:23][CH2:24][C:25]([F:27])([F:28])[F:26])=[CH:19][CH:18]=2)[C:12](=[O:16])[C:13]2[CH2:14][CH2:15][NH:6][C:7](=[O:32])[C:8]=2[N:9]=1)[CH3:31]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 866853887-(2,4-Dimethoxybenzyl)-2-(ethylsulfanyl)-3-[4-(2,2,2-trifluoroethoxy)phenyl]-3,5,6,7-tetrahydropyrido[3,4-d]pyrimidine-4,8-dione

생성물 1

HCID 680153252-(Ethylsulfanyl)-3-[4-(2,2,2-trifluoroethoxy)phenyl]-3,5,6,7-tetrahydropyrido[3,4-d]pyrimidine-4,8-dione수율 73.6%

시약·촉매·용매 1

HCID 284Formic Acid용매

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온도
100 °C

실험 절차

7-(2,4-Dimethoxybenzyl)-2-(ethylsulfanyl)-3-[4-(2,2,2-trifluoroethoxy)phenyl]-3,5,6,7-tetrahydropyrido[3,4-d]pyrimidine-4,8-dione (71 mg) was dissolved in formic acid (3 ml), and the solution was stirred at 100° C. for 1 hr, allowed to be cooled to room temperature, and concentrated under reduced pressure. The residue was subjected to azeotropic distillation with toluene. The obtained white solid was purified by silica gel column chromatography (methanol/ethyl acetate) to give the title compound (38 mg) as a white solid.

후처리

  1. temperatureto be cooled to room temperature
  2. concentrationconcentrated under reduced pressure
  3. distillationThe residue was subjected to azeotropic distillation with toluene
  4. customThe obtained white solid was purified by silica gel column chromatography (methanol/ethyl acetate)

출처 및 근거

ORD 기록
ord-b37c9c30c8fd4dbd9fe61323d2d6254d
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09023858B2

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