Propargyl alcohol → HCID 15045667, 화합물

HRID 1460283

반응식

HRID 1460283 반응식
[CH2:1]([C:16]1[CH:17]=[C:18]([OH:22])[CH:19]=[CH:20][CH:21]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15].[CH2:23](O)[C:24]#[CH:25].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCC)=O)=NC(OCC)=O>O.CCCCCC>[CH2:1]([C:16]1[CH:17]=[C:18]([O:22][CH2:25][C:24]#[CH:23])[CH:19]=[CH:20][CH:21]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15]

참가 물질

7

반응물 4

HCID 7859Propargyl alcoholHCID 11776TriphenylphosphineHCID 68146Hydrogenated cardanolHCID 220568ethyl N-ethoxycarbonyliminocarbamate

생성물 1

HCID 15045667HCID 15045667, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8058Hexane용매

실험 절차

To a solution of 24.4 g (80 mmol) of 3-pentadecylphenol, 4.93 g (88 mmol) of propargyl alcohol and 23.1 g (88 mmol) of triphenylphosphine cooled to 15° C. is added dropwise 15.3 g (13.9 ml, 88 mmol) of diethyl azodicarboxylate. The mixture is stirred for 4.5 hours and then is diluted with water and extracted with hexane (3 times). The hexane extracts are combined, washed with 1N sodium hydroxide and are dried over magnesium sulfate overnight. Filtration and evaporation gives crude oil which is subjected to flash chromatography using hexane as eluting solvent. The appropriate fractions are combined to give the title compound as an oil which solidifies upon standing: mp. 26°-27° C. The product is used without further characterization.

후처리

  1. extractionextracted with hexane (3 times)
  2. washwashed with 1N sodium hydroxide
  3. dry with materialare dried over magnesium sulfate overnight
  4. filtrationFiltration and evaporation
  5. customgives crude oil which
  6. washas eluting solvent

출처 및 근거

ORD 기록
ord-d6b9cf94a0484c3b9e6002f1a161c67e
출처 데이터셋
uspto-grants-1991_12
특허 번호
US05070207

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