1-Decanol → (6-n-Decyloxy-2-naphthyl)propanonitrile

HRID 372928

반응식

HRID 372928 반응식
[OH:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[CH:8]=[C:7]([CH:12]([CH3:15])[C:13]#[N:14])[CH:6]=[CH:5]2.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCC)=O)=NC(OCC)=O.[CH2:47](O)[CH2:48][CH2:49][CH2:50][CH2:51][CH2:52][CH2:53][CH2:54][CH2:55][CH3:56]>C1COCC1>[CH2:47]([O:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[CH:8]=[C:7]([CH:12]([CH3:15])[C:13]#[N:14])[CH:6]=[CH:5]2)[CH2:48][CH2:49][CH2:50][CH2:51][CH2:52][CH2:53][CH2:54][CH2:55][CH3:56]

참가 물질

6

반응물 4

HCID 81741-DecanolHCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 19097091(6-Hydroxy-2-naphthyl)-propanonitrile

생성물 1

HCID 67849695(6-n-Decyloxy-2-naphthyl)propanonitrile

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
5 °C

실험 절차

Into 20 ml of dry THF, were dissolved 1.5 g of oa (6-hydroxy-2-naphthyl)-propanonitrile and 3.0 g of triphenylphosphine, and cooled to 5° C. To this solution, were added dropwise 2.0 g of diethyl azodicarboxylate and then 1.2 g of n-decyl alcohol, and stirred at room temperature for 12 hours. The resulting reaction mixture was extracted with ether, followed by washing three times the ether phase with water and then distilling off the ether. The resulting oily product was extracted with hexane, and the hexanesoluble matter was recrystallized with methanol to obtain 0.7 g of oa (6-n-decyloxy-2-naphthyl)propanonitrile (Compound No. 1-10) of this invention.

후처리

  1. customThe resulting reaction mixture
  2. extractionwas extracted with ether
  3. washby washing three times the ether phase with water
  4. distillationdistilling off the ether
  5. extractionThe resulting oily product was extracted with hexane
  6. customthe hexanesoluble matter was recrystallized with methanol

출처 및 근거

ORD 기록
ord-842523f6f5274584a748f187a6a500e1
출처 데이터셋
uspto-grants-1992_11
특허 번호
US05160662

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