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m-Chloroperbenzoic acid → HCID 178502003, 화합물

HRID 464784
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HRID 464784 반응식
[NH2:1][C:2]1[N:7]=[C:6]([NH:8][C:9]([O:11][CH3:12])=[O:10])[CH:5]=[C:4]([O:13][S:14]([C:17]2[CH:22]=[CH:21][C:20]([CH3:23])=[CH:19][CH:18]=2)(=[O:16])=[O:15])[N:3]=1.ClC1C=CC=C(C(OO)=[O:32])C=1>C(Cl)Cl.CO>[NH2:1][C:2]1[N+:7]([O-:32])=[C:6]([NH:8][C:9]([O:11][CH3:12])=[O:10])[CH:5]=[C:4]([O:13][S:14]([C:17]2[CH:22]=[CH:21][C:20]([CH3:23])=[CH:19][CH:18]=2)(=[O:16])=[O:15])[N:3]=1
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반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 12857764Methyl 2-amino-6-[(p-tolylsulfonyl)oxy]-4-pyrimidinecarbamate

생성물 1

HCID 178502003HCID 178502003, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

350 g of methyl 2-amino-6-[(p-tolylsulfonyl)oxy]-4-pyrimidinecarbamate are suspended in 6.3 l of methylene chloride and 1 l of methanol. At room temperature there are added thereto 370 g of m-chloroperbenzoic acid and the mixture is stirred for a further 16 hours. The yellowish solution is subsequently extracted with 3 l of 2N soda solution. The aqueous phase is extracted with 1 l of methylene chloride. The combined organic phases are washed with 2 l of water and evaporated in vacuo. The crystalline residue is suspended in 1.5 l of ether while stirring. The pale yellowish crystals are filtered off under suction and washed with 0.5 l of ether. After drying at 40° in vacuo, there is obtained methyl 2-amino-6-[(p-tolylsulfonyl)oxy]-4-pyrimidinecarbamate-3-oxide.

후처리

  1. additionAt room temperature there are added
  2. extractionThe yellowish solution is subsequently extracted with 3 l of 2N soda solution
  3. extractionThe aqueous phase is extracted with 1 l of methylene chloride
  4. washThe combined organic phases are washed with 2 l of water
  5. customevaporated in vacuo
  6. filtrationThe pale yellowish crystals are filtered off under suction
  7. washwashed with 0.5 l of ether
  8. customAfter drying at 40° in vacuo

출처 및 근거

ORD 기록
ord-04d4688b5ef24524bd2d281d4d537b31
출처 데이터셋
uspto-grants-1985_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04549019

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