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

HRID 1283837ノート

反応式

HRID 1283837 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-86596acdeb1f4ef388dba2a992ce8665
出典データセット
uspto-grants-1976_08
特許番号
US03976661

反応ノート

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