HCID 13999247, 화합물 → 2-Ethyl-2-methylbutyric acid

HRID 1165110

반응식

HRID 1165110 반응식
[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]

참가 물질

4

반응물 2

HCID 13999247HCID 13999247, 화합물HCID 23668193Sodium Nitrite

생성물 1

HCID 298462-Ethyl-2-methylbutyric acid

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
50 °C

실험 절차

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).

후처리

  1. additionwere added dropwise to the resulting suspension

출처 및 근거

ORD 기록
ord-3789f7b1958042fbb2412a0d9ee6956a
출처 데이터셋
uspto-grants-1990_03
특허 번호
US04908138

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