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

HRID 485981

反応式

HRID 485981 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
5 °C

実験手順

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 hexane-soluble 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.

後処理

  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 hexane-soluble matter was recrystallized with methanol

出典と根拠

ORDレコード
ord-3ec1c237d76d406ea5578f0b330c40b6
出典データセット
uspto-grants-1994_03
特許番号
US05290478

関連ノート

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