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Hydrochloric Acid → N,N,N'-trimethyl-N'-(6-dimethylaminomethyl-2-pyridyl)urea hydrochloride hemihydrate

HRID 1154696
ノート
印刷プレビュー

反応式

HRID 1154696 の反応式
[CH3:1][N:2]([CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([NH:11][CH3:12])[N:6]=1)[CH3:3].C(N(CC)CC)C.[CH3:20][N:21]([CH3:25])[C:22]([Cl:24])=[O:23].[ClH:26]>C1C=CC=CC=1>[OH2:23].[ClH:24].[CH3:20][N:21]([CH3:25])[C:22]([N:11]([CH3:12])[C:7]1[CH:8]=[CH:9][CH:10]=[C:5]([CH2:4][N:2]([CH3:3])[CH3:1])[N:6]=1)=[O:23].[CH3:20][N:21]([CH3:25])[C:22]([N:11]([C:7]1[CH:8]=[CH:9][CH:10]=[C:5]([CH2:4][N:2]([CH3:1])[CH3:3])[N:6]=1)[CH3:12])=[O:23].[ClH:26]
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 313Hydrochloric Acid2 回HCID 6598Dimethylcarbamoyl ChlorideHCID 8471TriethylamineHCID 20434276N,N-dimethyl-6-(methylamino)-2-Pyridinemethanamine

生成物 1

HCID 70505628N,N,N'-trimethyl-N'-(6-dimethylaminomethyl-2-pyridyl)urea hydrochloride hemihydrate

試薬・触媒・溶媒 1

HCID 241
Benzene
溶媒

実験手順

To 2-dimethylaminomethyl-6-methylaminopyridine (2.14 g, 0.013 mol) in dry benzene (35 ml) is added triethylamine (1.77 g, 0.0175 mol) and dimethylcarbamoyl chloride (1.72 g, 0.016 mol). The solution is stirred under nitrogen at reflux for 16 hours overnight. The mixture is cooled to room temperature and filtered. The filtrate is concentrated in vacuo and the residual oil is taken up in ether, filtered and again concentrated in vacuo. The residual oil is converted to the monohydrochloride salt with 6N ethanolic hydrochloric acid (1.7 ml, 0.0103 mol). The solid is recrystallized from ethanol-ether several times, affording 2.2 g of N,N,N'-trimethyl-N'-(6-dimethylaminomethyl-2-pyridyl)urea hydrochloride hemihydrate as a white solid, m.p. 154°-155° C.

後処理

  1. temperatureat reflux for 16 hours overnight
  2. filtrationfiltered
  3. concentrationThe filtrate is concentrated in vacuo
  4. filtrationfiltered
  5. concentrationagain concentrated in vacuo
  6. customThe solid is recrystallized from ethanol-ether several times

出典と根拠

ORDレコード
ord-d7b0bfe92a9d4c9da209568a767457c9
出典データセット
uspto-grants-1984_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04490533

反応ノート

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