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Dimethylamine → 4-(3-Buten-1-yl)-6-(dimethylamino)-2-hydrazino-1,3,5-triazine

HRID 1786115
ノート
印刷プレビュー

反応式

HRID 1786115 の反応式
[N:1]1[C:8](Cl)=[N:7][C:5](Cl)=[N:4][C:2]=1Cl.[CH2:10]([Mg]Br)[CH2:11][CH:12]=[CH2:13].C[CH2:17][N:18]([CH:22](C)C)C(C)C.CNC.O.[NH2:29][NH2:30]>C1C=CC=CC=1.O1CCOCC1>[CH2:10]([C:2]1[N:4]=[C:5]([N:18]([CH3:22])[CH3:17])[N:7]=[C:8]([NH:29][NH2:30])[N:1]=1)[CH2:11][CH:12]=[CH2:13]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 674DimethylamineHCID 7954Cyanuric chlorideHCID 24654Hydrazine hydrate (1:1)HCID 81531DiisopropylethylamineHCID 178418797HCID 178418797、化合物

生成物 1

HCID 688481234-(3-Buten-1-yl)-6-(dimethylamino)-2-hydrazino-1,3,5-triazine

試薬・触媒・溶媒 2

HCID 241
Benzene
溶媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
0 °C

実験手順

To a cyanuric chloride (1.07 g, 5.80 mmol) in anhydrous benzene (10.7 mL) was added at 0° C. dropwise a solution of 3-butenylmagnesium bromide (0.5M in THF, 12.8 mL, 6.38 mmol). The resulting mixture was stirred at 0° C. for 3 hrs. To the mixture were added 1,4-dioxane (10 mL), DIPEA (1.1 mL), followed by addition of dimethylamine (2.0M in MeOH, 3.2 mL, 6.38 mmol) at 0° C. The mixture was stirred and allowed to warm up to room temperature over 2 hours. Finally to it was added hydrazine hydrate (7.0 mL) at room temperature. The mixture was stirred at room temperature overnight. Then the volatiles were evaporated in vacuo. The residue was purified by HPLC to provide the title compound as a white solid. MH+209.

後処理

  1. stirringThe mixture was stirred
  2. temperatureto warm up to room temperature over 2 hours
  3. stirringThe mixture was stirred at room temperature overnight
  4. customThen the volatiles were evaporated in vacuo
  5. customThe residue was purified by HPLC

出典と根拠

ORDレコード
ord-df1d91d0ebde4ebe867f1af20cecb905
出典データセット
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07507726B2

反応ノート

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