Ethyl Acetoacetate → HCID 178472877, 화합물

HRID 75488노트

반응식

HRID 75488 반응식
[C:1]([O:7][CH2:8][CH3:9])(=[O:6])[CH2:2][C:3]([CH3:5])=[O:4].[N:10]([O-])=[O:11].[Na+]>C(O)(=O)C.O>[OH:11][N:10]=[C:2]([C:3](=[O:4])[CH3:5])[C:1]([O:7][CH2:8][CH3:9])=[O:6]

참가 물질

5

반응물 2

HCID 8868Ethyl Acetoacetate2회HCID 23668193Sodium Nitrite

생성물 1

HCID 178472877HCID 178472877, 화합물

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매2회

실험 절차

To a solution of ethyl acetoacetate (compound 7, 30 g, 0.23 mol) in acetic acid (35 mL) was added slowly sodium nitrite (18.0 g, 0.25 mol) in cold water (40 mL) at −10° C. The reaction mixture was stirred for 1 hr, then added cold water (120 mL) and stirred for 3 hrs. The mixture was extracted with diethyl ether (300 mL). The organic layer was washed with saturated NaHCO3 (400 mL×2), then dried over anhydrous MgSO4, filtered and concentrated in vacuo. The obtained product (21.46 g, white solid) was used for the next step without purification.

후처리

  1. stirringstirred for 3 hrs
  2. extractionThe mixture was extracted with diethyl ether (300 mL)
  3. washThe organic layer was washed with saturated NaHCO3 (400 mL×2)
  4. dry with materialdried over anhydrous MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe obtained product (21.46 g, white solid) was used for the next step without purification

출처 및 근거

ORD 기록
ord-38b8e18b3cb54831ab47c0f5dcaddc64
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08835436B2

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