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Acetic Anhydride → 2-Acetamido-4-methyl-6-benzyloxypyrimidine

HRID 2058165
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HRID 2058165 반응식
[C:1](OC(=O)C)(=[O:3])[CH3:2].[NH2:8][C:9]1[N:14]=[C:13]([CH3:15])[CH:12]=[C:11]([O:16][CH2:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[N:10]=1.C(=O)([O-])[O-].[Na+].[Na+]>C1C=CC=CC=1>[C:1]([NH:8][C:9]1[N:14]=[C:13]([CH3:15])[CH:12]=[C:11]([O:16][CH2:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[N:10]=1)(=[O:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 10340Sodium CarbonateHCID 233498922-Amino-4-methyl-6-benzyloxypyrimidine

생성물 1

HCID 233499132-Acetamido-4-methyl-6-benzyloxypyrimidine

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

Acetic anhydride (15.3 g, 0.15 mole) is added to a stirred suspension of 2-amino-4-methyl-6-benzyloxypyrimidine (23.6 g, 0.11 mole) in 150 ml of benzene. The mixture is heated at reflux for 4 hours. It is cooled, neutralized with aqueous sodium carbonate and the benzene layer separated. The benzene solution is concentrated under vacuum to an oil from which 2-acetamido-4-methyl-6-benzyloxy-pyrimidine melting at 121°-122° C. is isolated by crystallization from hexane n-butyl chloride.

후처리

  1. temperatureThe mixture is heated
  2. temperatureat reflux for 4 hours
  3. temperatureIt is cooled
  4. customthe benzene layer separated
  5. concentrationThe benzene solution is concentrated under vacuum to an oil from which 2-acetamido-4-methyl-6-benzyloxy-pyrimidine melting at 121°-122° C.
  6. customis isolated by crystallization from hexane n-butyl chloride

출처 및 근거

ORD 기록
ord-03810d6e3c884d65a1674969fd0bdb74
출처 데이터셋
uspto-grants-1980_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04215121

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