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Hexane → HCID 178502003, 화합물

HRID 464777
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HRID 464777 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.CCCCCC>CO.C(Cl)Cl>[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 8058HexaneHCID 70297m-Chloroperbenzoic acid2회HCID 12857764Methyl 2-amino-6-[(p-tolylsulfonyl)oxy]-4-pyrimidinecarbamate

생성물 1

HCID 178502003HCID 178502003, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

20.6 g of methyl 2-amino-6-[(p-tolylsulphonyl)oxy]-4-pyrimidinecarbamate are suspended in 120 ml of methanol and 720 ml of methylene chloride. While stirring there are added thereto at room temperature 20.5 g of m-chloroperbenzoic acid and after 6 hours a further 16.3 g of m-chloroperbenzoic acid. The mixture is stirred overnight and subsequently treated with 1.5 l of hexane, whereby a precipitate separates. The precipitate is filtered off under suction and dried, there being obtained crude methyl 2-amino-6-[(p-tolylsulfonyl)oxy]-4-pyrimidinecarbamate-3-oxide of melting point 139°-142°.

후처리

  1. additionare added
  2. stirringThe mixture is stirred overnight
  3. filtrationThe precipitate is filtered off under suction
  4. customdried

출처 및 근거

ORD 기록
ord-1b08ea11b6154ceda5802aab7b982de4
출처 데이터셋
uspto-grants-1985_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04549019

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