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2-Chloroethanol → 1-(2-Hydroxyethyl)-3,5,6-trimethylpyrazin-2-one

HRID 1904326
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HRID 1904326 반응식
[OH:1][C:2]1[C:7]([CH3:8])=[N:6][C:5]([CH3:9])=[C:4]([CH3:10])[N:3]=1.[OH-].[Na+].[C:13]([OH:17])(C)(C)[CH3:14].C(Cl)CO>O>[OH:17][CH2:13][CH2:14][N:3]1[C:4]([CH3:10])=[C:5]([CH3:9])[N:6]=[C:7]([CH3:8])[C:2]1=[O:1]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 342-ChloroethanolHCID 6386tert-ButanolHCID 14798Sodium HydroxideHCID 178432813HCID 178432813, 화합물

생성물 1

HCID 147735301-(2-Hydroxyethyl)-3,5,6-trimethylpyrazin-2-one수율 79.1%

시약·촉매·용매 1

HCID 962Water용매

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온도
60 °C

실험 절차

2-Hydroxy-3,5,6-trimethylpyrazine (13.8 g, 0.1M) and 5N NaOH (100 ml, 0.5M) were added to t-butanol (200 ml). Ethylene chlorohydrin (40.3 g, 0.5M) was added thereto and the mixture was stirred at 60° C. for 2 hours. Water was added to the reaction mixture, which was then extracted 10 times with chloroform (100 ml), and the extract dried with anhydrous magnesium sulfate and concentrated in vacuo. The residue was charged on a column of silica-gel (Wako Pure Chem. Co., C-200) and eluted with chloroform-methanol (300:1) to obtain the product (14.4 g, yield: 79.1%).

후처리

  1. extractionwas then extracted 10 times with chloroform (100 ml)
  2. dry with materialthe extract dried with anhydrous magnesium sulfate
  3. concentrationconcentrated in vacuo
  4. additionThe residue was charged on a column of silica-gel (Wako Pure Chem. Co., C-200)
  5. washeluted with chloroform-methanol (300:1)

출처 및 근거

ORD 기록
ord-290968a95535432492158b90947c070a
출처 데이터셋
uspto-grants-1989_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04837319

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