Sodium Nitrite → HCID 86718008, 화합물

HRID 1500470노트

반응식

HRID 1500470 반응식
[CH3:1][C@@H:2]1[CH2:6][C:5]2[CH:7]=[C:8]([CH3:11])[CH:9]=[CH:10][C:4]=2[O:3]1.[N:12]([O-:14])=[O:13].[Na+]>C(O)(C(F)(F)F)=O>[CH3:1][C@@H:2]1[CH2:6][C:5]2[CH:7]=[C:8]([CH3:11])[CH:9]=[C:10]([N+:12]([O-:14])=[O:13])[C:4]=2[O:3]1

참가 물질

4

반응물 2

HCID 23668193Sodium NitriteHCID 86718007HCID 86718007, 화합물

생성물 1

HCID 86718008HCID 86718008, 화합물

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

반응 조건

온도
0 °C

실험 절차

A mixture of (R)-2,5-dimethyl-2,3-dihydrobenzofuran (3d) (2.0 g, 13 mmol) in TFA (40 mL) was cooled to 0° C., NaNO2 (1.7 g, 23 mmol) was added thereto. It was stirred at ambient temperature for 12 h. The mixture was concentrated, poured into water (50 mL), extracted with EtOAc (150 mL), washed with brine, dried and concentrated. The residue was purified by column chromatography on silica gel eluting with hexanes/EtOAc (20:1) to give the title compound (3e).

후처리

  1. concentrationThe mixture was concentrated
  2. additionpoured into water (50 mL)
  3. extractionextracted with EtOAc (150 mL)
  4. washwashed with brine
  5. customdried
  6. concentrationconcentrated
  7. customThe residue was purified by column chromatography on silica gel eluting with hexanes/EtOAc (20:1)

출처 및 근거

ORD 기록
ord-b6a2dfdc30224808820956b1bf791b10
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09206166B2

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