反応式
[CH2:1]([C:3]([CH3:19])([CH2:17][CH3:18])[C:4](=[O:16])CC(N)(P(O)(=O)O)P(O)(=O)O)[CH3:2].N([O-])=[O:21].[Na+]>O>[CH2:17]([C:3]([CH3:19])([CH2:1][CH3:2])[C:4]([OH:16])=[O:21])[CH3:18]参加物
反応条件
- 温度
- 50 °C
実験手順
0.20 mol (63.4 g) 4-ethyl-4-methyl-3-oxo-1-aminohexane-1,1-di-phosphonic acid (IV) R2 =R3 =CH2CH3, R4 =CH3) were suspended in 600 ml 2N hydrochloric acidd and a solution of 0.8 mol (55.2 g) sodium nitrite dissolved in 1104 ml water were added dropwise to the resulting suspension with stirring over a period of 7 hours at 50° C. 2-Ethyl-2-methyl-butyric acid was formed as the organic phase and was extracted with ether. Unused nitrous acid was removed with hydrazine before working up. The aqueous phase was concentrated to around 300 ml in a rotary evaporator and alkylized to pH 9 with sodium hydroxide. The tetrasodium salt of hydroxyacetonitrile diphosphonic acid (III, M=Na) crystallized out from the cold solution in the form of the octahydrate. The yield comprised 65% (58.4 g).
後処理
- additionwere added dropwise to the resulting suspension
出典と根拠
- ORDレコード
- ord-3789f7b1958042fbb2412a0d9ee6956a
- 出典データセット
- uspto-grants-1990_03
- 特許番号
- US04908138
関連ノート
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