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Triethylamine → E-4-(Carbo-tert.-butoxy)-4'-(4-carbo-tert.-butoxystyryl)tolan

HRID 974215
ノート
印刷プレビュー

反応式

HRID 974215 の反応式
CCN(CC)CC.Br[C:9]1[CH:14]=[CH:13][C:12]([CH:15]=[CH:16][C:17]2[CH:22]=[CH:21][C:20]([C:23]([O:25][C:26]([CH3:29])([CH3:28])[CH3:27])=[O:24])=[CH:19][CH:18]=2)=[CH:11][CH:10]=1.[C:30]([O:34][C:35](=[O:44])[C:36]1[CH:41]=[CH:40][C:39]([C:42]#[CH:43])=[CH:38][CH:37]=1)([CH3:33])([CH3:32])[CH3:31]>C(#N)C.[Cu]I>[C:35]([C:36]1[CH:41]=[CH:40][C:39]([C:42]#[C:43][C:9]2[CH:14]=[CH:13][C:12](/[CH:15]=[CH:16]/[C:17]3[CH:22]=[CH:21][C:20]([C:23]([O:25][C:26]([CH3:29])([CH3:28])[CH3:27])=[O:24])=[CH:19][CH:18]=3)=[CH:11][CH:10]=2)=[CH:38][CH:37]=1)([O:34][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:44]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 8471TriethylamineHCID 13965008Tert-butyl 4-ethynylbenzoateHCID 573054164-Bromo-4'-carbo-tert.-butoxystilbene

生成物 1

HCID 131717083E-4-(Carbo-tert.-butoxy)-4'-(4-carbo-tert.-butoxystyryl)tolan

試薬・触媒・溶媒 2

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)触媒
HCID 6342
Acetonitrile
溶媒
2 回

実験手順

300 ml of NEt3 and 20.46 g of Pφ3 are added under nitrogen to 234 g of 4-bromo-4'-carbo-tert.-butoxystilbene in 1 l of absolute acetonitrile. Nitrogen is passed through the stirred suspension for 20 minutes and 9.12 g of (Pφ3)2PdCl2 and 2.5 g of copper(I)iodide are then added. 144 g of 4-Ethinyl benzoic acid tert.-butyl ester dissolved in 1 l of absolute acetonitrile are then added dropwise under reflux over a period of 6 hours and the reaction mixture is boiled under reflux overnight. The hot product obtained after suction filtration is dissolved in CH2Cl2, washed several times with H2O and dried and the solvent is removed.

後処理

  1. additionare then added dropwise
  2. temperatureunder reflux over a period of 6 hours
  3. temperatureunder reflux overnight
  4. customThe hot product obtained
  5. filtrationafter suction filtration
  6. dissolutionis dissolved in CH2Cl2
  7. washwashed several times with H2O
  8. customdried
  9. customthe solvent is removed

出典と根拠

ORDレコード
ord-55e7a4ee3d36431cac4a797bb1cca528
出典データセット
uspto-grants-1991_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05068300

反応ノート

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