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Hydrochloric Acid → HCID 178432663, 화합물

HRID 1886075
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HRID 1886075 반응식
[CH3:1][C:2]1[N:3]=[C:4]([CH3:28])[C:5]2[CH:11]=[CH:10][C:9](=[O:12])[N:8]([CH2:13][C:14]3[CH:19]=[CH:18][C:17]([C:20]4[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=4[C:26]#[N:27])=[CH:16][CH:15]=3)[C:6]=2[N:7]=1.[N-:29]=[N+:30]=[N-:31].[Na+].C([Sn](Cl)(CCCC)CCCC)CCC.Cl>>[CH3:1][C:2]1[N:3]=[C:4]([CH3:28])[C:5]2[CH:11]=[CH:10][C:9](=[O:12])[N:8]([CH2:13][C:14]3[CH:19]=[CH:18][C:17]([C:20]4[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=4[C:26]4[NH:31][N:30]=[N:29][N:27]=4)=[CH:16][CH:15]=3)[C:6]=2[N:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 313Hydrochloric AcidHCID 15096Tributyltin ChlorideHCID 33557Sodium AzideHCID 10690257HCID 10690257, 화합물

생성물 1

HCID 178432663HCID 178432663, 화합물

실험 절차

Using the same procedure as described in Step 3 of Example 8, heat a mixture of 2,4-dimethyl-8-[[2'-cyano[1,1-biphenyl]-4-yl]methyl]-7H-pyrido[2,3-d]pyrimidin-7-one, NaN3, and tri-n-butyltin chloride in xylenes under reflux for 48 h. Cool the mixture and add 1N HCl (2 mL). Add CHCl3 and water, and dry (MgSO4) and concentrate the organic phase. Recrystallization from EtOAc gives the product.

후처리

  1. temperatureheat
  2. temperatureunder reflux for 48 h
  3. temperatureCool the mixture
  4. dry with materialAdd CHCl3 and water, and dry (MgSO4)
  5. concentrationconcentrate the organic phase
  6. customRecrystallization from EtOAc
  7. customgives the product

출처 및 근거

ORD 기록
ord-132102d57a7a40799dc56511169c204c
출처 데이터셋
uspto-grants-1992_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05149699

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