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Ethanol → HCID 178419517, 화합물

HRID 633709
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HRID 633709 반응식
[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
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참가 물질

6

반응물 3

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

생성물 1

HCID 178419517HCID 178419517, 화합물수율 57.2%

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 6344Dichloromethane용매

실험 절차

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:

후처리

  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

출처 및 근거

ORD 기록
ord-101d3024cb0a45089a4a268c4a6dbfc9
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09321790B2

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