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Sodium Nitrite → HCID 178504894, 화합물

HRID 2309576
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HRID 2309576 반응식
[Cl:1][CH2:2][C:3](=[O:14])[CH2:4][C:5]([O:7][CH2:8][CH2:9][S:10]([CH3:13])(=[O:12])=[O:11])=[O:6].[N:15]([O-])=[O:16].[Na+]>C(O)(=O)C.O>[Cl:1][CH2:2][C:3](=[O:14])[C:4](=[N:15][OH:16])[C:5]([O:7][CH2:8][CH2:9][S:10]([CH3:13])(=[O:12])=[O:11])=[O:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 23668193Sodium NitriteHCID 543240772-(Methanesulfonyl)ethyl 4-chloro-3-oxobutanoate

생성물 1

HCID 178504894HCID 178504894, 화합물수율 85%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

실험 절차

In 315 ml of glacial acetic acid was suspended 156.3 g (0.644 mole) of methylsulfonylethyl 4-chloroacetoacetate as obtained in Example 1. The suspension was cooled to 5° C. or below and a solution of 44.4 g (0.644 mole) of sodium nitrite in 140 ml of water was added at 0°-5° C. over a period of about 2 hours. The mixture was stirred for 30 minutes, poured in ice water and extracted with ethyl acetate. The organic layer was washed with water and dried over anhydrous sodium sulfate. The solvent was then distilled off to give 148.7 g of methylsulfonylethyl 4-chloro-2-hydroxyiminoacetoacetate as an oil.

후처리

  1. customas obtained in Example 1
  2. temperatureThe suspension was cooled to 5° C. or below
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationThe solvent was then distilled off

출처 및 근거

ORD 기록
ord-b338687a9ef645b9ba290d76968ed610
출처 데이터셋
uspto-grants-1987_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04695639

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