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

HRID 1288270
ノート
印刷プレビュー

反応式

HRID 1288270 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-944bb8efc4e444de95138e12ee6b9149
出典データセット
uspto-grants-1976_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03987160

反応ノート

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