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Sodium Sulfite → Acetic acid, chloro(diethoxyphosphinyl)-, 1,1-dimethylethyl ester

HRID 1870540
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HRID 1870540 반응식
[Cl:1][C:2](Cl)([P:10]([O:15][CH2:16][CH3:17])([O:12][CH2:13][CH3:14])=[O:11])[C:3]([O:5][C:6]([CH3:9])([CH3:8])[CH3:7])=[O:4].S([O-])([O-])=O.[Na+].[Na+]>C(O)C.O>[Cl:1][CH:2]([P:10]([O:15][CH2:16][CH3:17])([O:12][CH2:13][CH3:14])=[O:11])[C:3]([O:5][C:6]([CH3:9])([CH3:8])[CH3:7])=[O:4]
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참가 물질

5

반응물 2

HCID 24437Sodium SulfiteHCID 53950305HCID 53950305, 화합물

생성물 1

HCID 10902235Acetic acid, chloro(diethoxyphosphinyl)-, 1,1-dimethylethyl ester수율 100%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

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온도
0 °C

실험 절차

The title compound of Step B (18.4 g, 0.0572 mol) was dissolved in ethanol (140 mL) and cooled to 0° C. A solution of sodium sulfite (14.4 g, 0.1144 mol) in H2O (63 mL) was added with stirring such that the internal temperature remained below 14° C. The cooling bath was removed and the mixture was stirred at room temperature for 30 min. The reaction mixture was extracted five times with chloroform, and the combined organic phase was dried (MgSO4), filtered and concentrated to afford 16.4 g of the title compound of Step C as a clear oil. 1H NMR (300 MHz, CDCl3): δ 4.43 (d,1H, J=15.9 Hz), 4.30-4.24 (m,4H), 1.52 (s,9H), 1.38 (t,6H, J=6.9 Hz).

후처리

  1. customremained below 14° C
  2. customThe cooling bath was removed
  3. stirringthe mixture was stirred at room temperature for 30 min
  4. extractionThe reaction mixture was extracted five times with chloroform
  5. dry with materialthe combined organic phase was dried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-4144914206334a05b7c7cd5a3e7488e6
출처 데이터셋
uspto-grants-2000_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06096895

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