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Ethanol → HCID 178419517、化合物

HRID 633709
ノート
印刷プレビュー

反応式

HRID 633709 の反応式
[N:1]#[C:2][Br:3].[F:4][C:5]([F:12])([F:11])[C@@:6]([CH3:10])([NH2:9])[CH2:7][NH2:8].C(O)C>ClCCl.C(#N)C>[BrH:3].[CH3:10][C@@:6]1([C:5]([F:12])([F:11])[F:4])[CH2:7][NH:8][C:2]([NH2:1])=[N:9]1
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 3

HCID 702EthanolHCID 10476Cyanogen BromideHCID 16083880(2S)-3,3,3-Trifluoro-2-methylpropane-1,2-diamine

生成物 1

HCID 178419517HCID 178419517、化合物収率 57.2%

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 6344Dichloromethane溶媒

実験手順

11.60 mL (34.90 mmol) of cyanogen bromide dissolved in dichloromethane are added portionwise to a solution, cooled to 4° C., of 4.50 g (31.70 mmol) of (S)-3,3,3-trifluoro-2-methylpropane-1,2-diamine in 20 mL of acetonitrile, while maintaining the temperature between 5 and 10° C. At the end of the addition, the reaction mixture is left at 5° C. for 30 minutes. The mixture obtained is then stirred at room temperature overnight. The resulting mixture is then concentrated under vacuum. The residue obtained is taken up twice with ethanol and then twice with toluene, and evaporated to dryness each time. The solid obtained is triturated with ethyl ether and then filtered off to give 4.50 g of (S)-4-methyl-4-trifluoromethyl-4,5-dihydro-1H-imidazol-2-ylamine hydrobromide in the form of a white solid, the characteristics of which are as follows:

後処理

  1. additionare added portionwise to a solution
  2. temperaturewhile maintaining the temperature between 5 and 10° C
  3. additionAt the end of the addition
  4. customThe mixture obtained
  5. concentrationThe resulting mixture is then concentrated under vacuum
  6. customThe residue obtained
  7. customtwice with toluene, and evaporated to dryness each time
  8. customThe solid obtained
  9. customis triturated with ethyl ether
  10. filtrationfiltered off

出典と根拠

ORDレコード
ord-101d3024cb0a45089a4a268c4a6dbfc9
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09321790B2

反応ノート

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