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Ammonium Chloride → 2,2,3-Trimethyl-4-(1,2,4-triazol-1-yl)-6-phenoxy-hexan-3-ol

HRID 1702152
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HRID 1702152 반응식
[CH3:1][C:2]([CH3:21])([C:4](=[O:20])[CH:5]([N:15]1[CH:19]=[N:18][CH:17]=[N:16]1)[CH2:6][CH2:7][O:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[CH3:3].[CH3:22][Mg]Br.[Cl-].[NH4+]>O1CCCC1>[CH3:3][C:2]([CH3:21])([C:4]([CH3:22])([OH:20])[CH:5]([N:15]1[CH:19]=[N:18][CH:17]=[N:16]1)[CH2:6][CH2:7][O:8][C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1)[CH3:1]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 128066802,2-Dimethyl-4-(1,2,4-triazol-1-yl)-6-phenoxy-hexan-3-oneHCID 178418573HCID 178418573, 화합물

생성물 1

HCID 205041962,2,3-Trimethyl-4-(1,2,4-triazol-1-yl)-6-phenoxy-hexan-3-ol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 6.0 g of 2,2-dimethyl-4-(1,2,4-triazol-1-yl)-6-phenoxy-hexan-3-one in 50 ml of tetrahydrofuran is added dropwise to a solution of 5.4 g of methyl-magnesium bromide in 28 ml of tetrahydrofuran, and after the slight exothermic reaction has subsided the mixture is left to stand for 24 hours at room temperature. It is then poured into 1,000 ml of 10% strength aqueous ammonium chloride solution and the batch is extracted twice with 200 ml of methylene chloride at a time. The organic phase is washed and dried over magnesium sulfate, and the methylene chloride is evaporated off under reduced pressure. 10 ml of diisopropyl ether are added to the residue, and 1.5 g of white crystals, of melting point 118°-120° C., are isolated from this mixture.

후처리

  1. customafter the slight exothermic reaction
  2. waitis left
  3. extractionthe batch is extracted twice with 200 ml of methylene chloride at a time
  4. washThe organic phase is washed
  5. dry with materialdried over magnesium sulfate
  6. customthe methylene chloride is evaporated off under reduced pressure
  7. addition10 ml of diisopropyl ether are added to the residue, and 1.5 g of white crystals, of melting point 118°-120° C.
  8. customare isolated from this mixture

출처 및 근거

ORD 기록
ord-a3275b9a6c02451db02e2009b3bd9b1e
출처 데이터셋
uspto-grants-1983_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04380546

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