Hydrochloric Acid → Dimethylamino-(1,4-dioxaspiro[4.5]dec-8-yl)-acetonitrile

HRID 12641노트

반응식

HRID 12641 반응식
[CH3:1][NH:2][CH3:3].[O:4]1[C:8]2([CH2:13][CH2:12][CH:11]([CH:14]=O)[CH2:10][CH2:9]2)[O:7][CH2:6][CH2:5]1.[C-:16]#[N:17].[K+].Cl>O.CO>[CH3:1][N:2]([CH:14]([CH:11]1[CH2:10][CH2:9][C:8]2([O:4][CH2:5][CH2:6][O:7]2)[CH2:13][CH2:12]1)[C:16]#[N:17])[CH3:3]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 674DimethylamineHCID 9032Potassium CyanideHCID 98989471,4-Dioxaspiro(4.5)decane-8-carbaldehyde

생성물 1

HCID 57839521Dimethylamino-(1,4-dioxaspiro[4.5]dec-8-yl)-acetonitrile

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

40% aqueous dimethylamine solution (85 ml, 0.67 mole), 1,4-dioxa-spiro-[4.5]decane-8-carbaldehyde 5 (240 g, 0.141 mole) and potassium cyanide (22.05 g, 0.338 mole) were added while cooling with ice to a mixture of 4N hydrochloric acid (37 ml) and methanol (22 ml). The mixture was stirred for four days at room temperature and then, after adding water (80 ml), extracted with diethyl ether (4×100 ml). The organic phase was dried over sodium sulfate, concentrated by evaporation in vacuo, and the product was obtained as a white solid.

후처리

  1. extractionextracted with diethyl ether (4×100 ml)
  2. dry with materialThe organic phase was dried over sodium sulfate
  3. concentrationconcentrated by evaporation in vacuo
  4. customthe product was obtained as a white solid

출처 및 근거

ORD 기록
ord-85f0a1c8da154ceeb53790dd29fb205d
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728028B2

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