2-Butanone oxime → HCID 86664633, 화합물

HRID 1183230

반응식

HRID 1183230 반응식
[CH3:1][C:2](=[N:5][OH:6])[CH2:3][CH3:4].[CH:7]1([N:13]=[C:14]=[N:15][CH:16]2[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]2)[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1>C1COCC1.[OH-].[Na+]>[CH:16]1([NH:15][C:14](=[N:13][CH:7]2[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]2)[O:6][N:5]=[C:2]([CH2:3][CH3:4])[CH3:1])[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21]1

참가 물질

5

반응물 2

HCID 72922-Butanone oximeHCID 10868Dicyclohexylcarbodiimide

생성물 1

HCID 86664633HCID 86664633, 화합물수율 76.6%

시약·촉매·용매 2

HCID 14798Sodium Hydroxide촉매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of methylethylketone oxime (4.6 g, 0.053 mol) in dry THF (30 ml) is added finely powdered NaOH (0.15 g) and dicyclohexylcarbodiimide (10.3 g, 0.05 mol). The mixture is then stirred 5 h at room temperature under argon. The turbid mixture is thereafter filtered and evaporated under reduced pressure. The residue is stirred 10 minutes with acetonitrile (30 ml), the acetonitrile phase is then discarded, the oily residue is dissolved in dichloromethane (30 ml), filtered and evaporated to afford 11.24 g of the title compound as a slightly yellow liquid.

후처리

  1. filtrationThe turbid mixture is thereafter filtered
  2. customevaporated under reduced pressure
  3. stirringThe residue is stirred 10 minutes with acetonitrile (30 ml)
  4. dissolutionthe oily residue is dissolved in dichloromethane (30 ml)
  5. filtrationfiltered
  6. customevaporated

출처 및 근거

ORD 기록
ord-f82b7ea3cd4e4be88badaef144abbde3
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08664288B2

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