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Acetic Acid → 2-(2-Allyloxyphenyl)-4,5-diaminopyrimid-6-one

HRID 1288270
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HRID 1288270 반응식
[CH2:1]([O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[C:11]1[NH:12][C:13](=[O:20])[C:14]([N:18]=O)=[C:15]([NH2:17])[N:16]=1)[CH:2]=[CH2:3].C(N(CC)CC)C.S(S([O-])=O)([O-])=O.[Na+].[Na+].C(O)(=O)C>O>[CH2:1]([O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[C:11]1[NH:12][C:13](=[O:20])[C:14]([NH2:18])=[C:15]([NH2:17])[N:16]=1)[CH:2]=[CH2:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 8471TriethylamineHCID 24489Sodium DithioniteHCID 1363546152-(2-Allyloxyphenyl)-4-amino-5-nitrosopyrimid-6-one

생성물 1

HCID 1360237872-(2-Allyloxyphenyl)-4,5-diaminopyrimid-6-one수율 85.3%

시약·촉매·용매 1

HCID 962Water
용매

실험 절차

2-(2-Allyloxyphenyl)-4-amino-5-nitrosopyrimid-6-one (6.3 g.) was suspended in a solution of triethylamine (15 ml.) in water (250 ml.). Sodium dithionite (12 g.) was added in portions with stirring at room temperature. The temperature of the mixture was then raised to 60° C., and it was stirred at this temperature for a further 20 minutes. The pH of the mixture was adjusted to 7 by the addition of glacial acetic acid, and the mixture cooled in ice/water. The solid was filtered off and washed with water to give 2-(2-allyloxyphenyl)-4,5-diaminopyrimid-6-one (5.1 g.), m.p. 127°-130° C.

후처리

  1. temperatureThe temperature of the mixture was then raised to 60° C.
  2. stirringit was stirred at this temperature for a further 20 minutes
  3. filtrationThe solid was filtered off
  4. washwashed with water

출처 및 근거

ORD 기록
ord-944bb8efc4e444de95138e12ee6b9149
출처 데이터셋
uspto-grants-1976_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03987160

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