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

HRID 1870540
ノート
印刷プレビュー

反応式

HRID 1870540 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 24437Sodium SulfiteHCID 53950305HCID 53950305、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-4144914206334a05b7c7cd5a3e7488e6
出典データセット
uspto-grants-2000_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06096895

反応ノート

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