Sodium borohydride → HCID 59226486, 화합물

HRID 1523413노트

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HRID 1523413 반응식
[N+:1]([C:4]1[CH:5]=[N:6][CH:7]=[CH:8][C:9]=1[C:10]1[CH2:15][CH2:14][CH2:13][C:12](=[O:16])[CH:11]=1)([O-:3])=[O:2].[BH4-].[Na+]>CCO>[N+:1]([C:4]1[CH:5]=[N:6][CH:7]=[CH:8][C:9]=1[C:10]1[CH2:15][CH2:14][CH2:13][CH:12]([OH:16])[CH:11]=1)([O-:3])=[O:2]

참가 물질

4

반응물 2

HCID 4311764Sodium borohydrideHCID 592265443-(3-Nitropyridin-4-yl)cyclohex-2-enone

생성물 1

HCID 59226486HCID 59226486, 화합물수율 99%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
0 °C

실험 절차

To a solution of 3-(3-nitropyridin-4-yl)cyclohex-2-enone (1.0 equiv.) was added EtOH (0.2 M) and CeCl3-7H2O (1.3 equiv.). The reaction was cooled to 0° C., then NaBH4 (1.3 equiv.) was added in portions. Stirred for 2 h at 0° C., then quenched by adding water, concentrated to remove the EtOH, added EtOAc, extracted the organics, dried with brine, then Na2SO4, and concentrated to yield 3-(3-nitropyridin-4-yl)cyclohex-2-enol (99%). LC/MS=221.1 (M+H), LC=2.235 min.

후처리

  1. customquenched
  2. additionby adding water
  3. concentrationconcentrated
  4. customto remove the EtOH
  5. additionadded EtOAc
  6. extractionextracted the organics,
  7. dry with materialdried with brine
  8. concentrationNa2SO4, and concentrated

출처 및 근거

ORD 기록
ord-9f067c43843d4bd09c85652c64b03b5f
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09079889B2

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