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Water → Benzyl [4-(4-chloropyrimidin-6-yloxy)-2,5-difluorophenyl]carbamate

HRID 2066284
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HRID 2066284 반응식
[CH2:1]([O:8][C:9](=[O:20])[NH:10][C:11]1[CH:16]=[C:15]([F:17])[C:14]([OH:18])=[CH:13][C:12]=1[F:19])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl:21][C:22]1[CH:27]=[C:26](Cl)[N:25]=[CH:24][N:23]=1.C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH2:1]([O:8][C:9](=[O:20])[NH:10][C:11]1[CH:16]=[C:15]([F:17])[C:14]([O:18][C:26]2[N:25]=[CH:24][N:23]=[C:22]([Cl:21])[CH:27]=2)=[CH:13][C:12]=1[F:19])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 709434,6-DichloropyrimidineHCID 57470872HCID 57470872, 화합물

생성물 1

HCID 57470873Benzyl [4-(4-chloropyrimidin-6-yloxy)-2,5-difluorophenyl]carbamate수율 89%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

Benzyl(2,5-difluoro-4-hydroxyphenyl)carbamate (4.90 g) was dissolved in N,N-dimethylformamide (30 ml), then 4,6-dichloropyrimidine (2.61 g) and potassium carbonate (3.63 g) were added thereto at room temperature, followed by stirring for 2 hr. Water (90 ml) was added to the reaction mixture to precipitate crystals. The crystals were collected by filtration and washed with water (30 ml, 6 times). The crystals were hot air-dried at 60° C. for 2 days to provide the titled compound as pale brown crystals (6.108 g, 89%).

후처리

  1. customat room temperature
  2. customto precipitate crystals
  3. filtrationThe crystals were collected by filtration
  4. washwashed with water (30 ml, 6 times)
  5. customThe crystals were hot air-dried at 60° C. for 2 days

출처 및 근거

ORD 기록
ord-a9b9d6933da74ae49ebfa1ff69be896e
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08288538B2

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