Triethylamine → [5,5-Dimethyl-1-(1-pyrrolidinyl)-1-cyclohexen-3-ylidene]-(dodecylsulfonyl)acetonitrile

HRID 1283837노트

반응식

HRID 1283837 반응식
Cl([O-])(=O)(=O)=O.Cl[C:7]1[CH2:12][C:11]([CH3:14])([CH3:13])[CH2:10][C:9](=[N+:15]2[CH2:19][CH2:18][CH2:17][CH2:16]2)[CH:8]=1.[CH2:20]([S:32]([CH2:35][C:36]#[N:37])(=[O:34])=[O:33])[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31].C(N(CC)CC)C>C(O)C>[CH3:13][C:11]1([CH3:14])[CH2:10][C:9]([N:15]2[CH2:19][CH2:18][CH2:17][CH2:16]2)=[CH:8][C:7](=[C:35]([S:32]([CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31])(=[O:34])=[O:33])[C:36]#[N:37])[CH2:12]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 104334(Dodecylsulphonyl)acetonitrileHCID 21516721N-(3-Chloro-5,5-dimethylcyclohex-2-en-1-ylidene)-pyrrolidinium perchlorate

생성물 1

HCID 53637640[5,5-Dimethyl-1-(1-pyrrolidinyl)-1-cyclohexen-3-ylidene]-(dodecylsulfonyl)acetonitrile

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

N-(3-Chloro-5,5-dimethylcyclohex-2-en-1-ylidene)-pyrrolidinium perchlorate (3.2 g.), dodecylsulfonylacetonitrile (2.7 g.) and triethylamine (3.1 ml.) are dissolved in ethanol (15 ml.) and heated at reflux for 5 minutes. After chilling, the solid is collected on a filter, washed with methanol and dried. Obtaining pure dye by recrystallization from methanol proved difficult. The product is eluted from basic alumina, using a 10% methanol-90% chloroform solvent mixture, and then recrystallized from methanol. The yield of purified dye is 0.5 g. (11%), m.p. 114°-115°C. This dye compound shows good ultraviolet absorption characteristics as indicated in the data in Table 1 below.

후처리

  1. temperatureheated
  2. temperatureat reflux for 5 minutes
  3. temperatureAfter chilling
  4. customthe solid is collected on a filter
  5. washwashed with methanol
  6. customdried
  7. customObtaining pure dye
  8. customby recrystallization from methanol proved difficult
  9. washThe product is eluted from basic alumina
  10. customrecrystallized from methanol
  11. customultraviolet absorption characteristics

출처 및 근거

ORD 기록
ord-86596acdeb1f4ef388dba2a992ce8665
출처 데이터셋
uspto-grants-1976_08
특허 번호
US03976661

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