Triethylamine → N-(adamantan-2-yl)prop-2-enamide

HRID 5497

반응식

HRID 5497 반응식
[C:1](Cl)(=[O:4])[CH:2]=[CH2:3].Cl.[CH:7]12[CH2:16][CH:11]3[CH2:12][CH:13]([CH2:15][CH:9]([CH2:10]3)[CH:8]1[NH2:17])[CH2:14]2.C(N(CC)CC)C>C(OCC)C.C(Cl)Cl>[CH:7]12[CH2:16][CH:11]3[CH2:12][CH:13]([CH2:15][CH:9]([CH2:10]3)[CH:8]1[NH:17][C:1](=[O:4])[CH:2]=[CH2:3])[CH2:14]2

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 13140Acryloyl chlorideHCID 253312-Aminoadamantane hydrochloride

생성물 1

HCID 14986569N-(adamantan-2-yl)prop-2-enamide

시약·촉매·용매 2

HCID 3283Diethyl Ether용매2회HCID 6344Dichloromethane용매

실험 절차

A solution of acryloyl chloride (4.52 g, 0.05 mole) in ethyl ether (20 ml) was added dropwise to a stirring mixture of 2-adamantylamine hydrochloride (9.35 g, 0.05 mole) and triethylamine (30.65 ml) in methylene chloride (200 ml) and ethyl ether (200 ml) over a 30 minute period. The solution was stirred for 12 hours, the solid filtered and washed with ethyl ether and the filtrate stripped to an oily material which was taken up in ethyl acetate and hexane and allowed to stand overnight. The solid was filtered, the filtrate concentrated and chilled and the product as an orange solid filtered and dried. The structure was confirmed by NMR.

후처리

  1. filtrationthe solid filtered
  2. washwashed with ethyl ether
  3. waitto stand overnight
  4. filtrationThe solid was filtered
  5. concentrationthe filtrate concentrated
  6. temperaturechilled
  7. filtrationthe product as an orange solid filtered
  8. customdried

출처 및 근거

ORD 기록
ord-2ab50f00f4ee40f3872001d53d2b0523
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05244899

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