Acetaldehyde → HCID 178477243、化合物

HRID 868490ノート

反応式

HRID 868490 の反応式
[Cl-].[Cl-].[CH:3]([O:6][Ti+2:7][O:8][CH:9]([CH3:11])[CH3:10])([CH3:5])[CH3:4].[CH:12](=[O:14])[CH3:13].C1C[O:18][CH2:17][CH2:16]1>>[CH:3]([O:6][Ti:7]([O:8][CH:9]([CH3:11])[CH3:10])([O:18][CH:17]=[CH2:16])[O:14][CH:12]=[CH2:13])([CH3:5])[CH3:4]

参加物

4

反応物 3

HCID 177AcetaldehydeHCID 8028Tetrahydrofuran2 回HCID 178460659HCID 178460659、化合物

生成物 1

HCID 178477243HCID 178477243、化合物

実験手順

Diisopropoxytitanium dichloride (0.262 g, 1.10 mmol) was dissolved in 20 ml of THF (dry, nitrogen atmosphere) in a 100 ml Schlenk flask. This solution was cooled to -78° C. at which point the lithium enolate of acetaldehyde, CH2 =CHOLi, in THF solution (2.20 mmol) was added to the stirred solution via syringe. This solution was allowed to warm to room temperature. After two hours of stirring, the solvent was evaporated by trap-to-trap distillation, leaving a yellow solid. This solid was extracted with pentane yielding a yellow pentane-soluble solid (crude yield 0.19 g, 70%). 1H NRM (CDCl3) δ 1.19 (d, J=6.4 Hz, 6.7H, CH--(CH3)2), 3.10 (d, J=28 Hz, 1H, OCH=CH2), 3.62 (s, 1H, OCH=CH2), 4.00 (sept, J=6.45 Hz, 1H, CH--(CH3)2), 6.55 (d, J=10.3 Hz, 1H, OCH=CH2), 7.01 (d, J=19.7, 1H, OCH=CH2).

後処理

  1. customthe solvent was evaporated by trap-to-trap
  2. distillationdistillation
  3. customleaving a yellow solid
  4. extractionThis solid was extracted with pentane yielding a yellow pentane-soluble solid (crude yield 0.19 g, 70%)

出典と根拠

ORDレコード
ord-4f35ce40b0c04908b6f0321fd4497b53
出典データセット
uspto-grants-1988_10
特許番号
US04780337

反応ノート

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