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Acetamide → 1,3,5-Triazine-2-carbonitrile, 4,6-dimethoxy-

HRID 2413076
ノート
印刷プレビュー

反応式

HRID 2413076 の反応式
[C-]#N.[K+].[C:4]([NH2:7])(=O)C.[Cl-].C[N+](C)(C)[C:11]1[N:16]=[C:15]([O:17][CH3:18])[N:14]=[C:13]([O:19][CH3:20])[N:12]=1>O>[C:4]([C:11]1[N:12]=[C:13]([O:19][CH3:20])[N:14]=[C:15]([O:17][CH3:18])[N:16]=1)#[N:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 178AcetamideHCID 9032Potassium CyanideHCID 131413314,6-Dimethoxy-N,N,N-trimethyl-1,3,5-triazin-2-aminium chloride

生成物 1

HCID 23202681,3,5-Triazine-2-carbonitrile, 4,6-dimethoxy-収率 38.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 26 g of potassium cyanide and 60 g of oven-dried acetamide was heated to 85°-90° C. To this melt was added 24 g of the product from Example 2 in portions over a period of 15-20 minutes. The resulting brown reaction solution was heated to 90°-100° C. for an additional one hour. When the solution had cooled to room temperature, water was added and the aqueous layer was extracted with ether and methylene chloride. The combined organic extracts were backwashed with several small portions of water, brine, and were then dried over magnesium sulfate and concentrated in vacuo to afford 6.5 g of 2-cyano-4,6-dimethoxy-1,3,5-triazine as a light yellow solid.

後処理

  1. temperaturewas heated to 85°-90° C
  2. temperatureThe resulting brown reaction solution was heated to 90°-100° C. for an additional one hour
  3. extractionthe aqueous layer was extracted with ether and methylene chloride
  4. dry with materialwere then dried over magnesium sulfate
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-232248879c4f4b3d86c8de105672fe7c
出典データセット
uspto-grants-1985_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04496392

反応ノート

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