Triethylamine → 1-[2,5-Dimethoxy-3,6-bis(methoxymethoxy)phenyl]-2-(2,2-dimethyl-4,6-dioxo-1,3-dioxan-5-ylidene)ethane

HRID 1588127ノート

反応式

HRID 1588127 の反応式
[CH3:1][O:2][C:3]1[C:8]([O:9][CH2:10][O:11][CH3:12])=[CH:7][C:6]([O:13][CH3:14])=[C:5]([O:15][CH2:16][O:17][CH3:18])[C:4]=1[CH2:19][CH:20]=O.[CH3:22][C:23]1([CH3:31])[O:30][C:28](=[O:29])[CH2:27][C:25](=[O:26])[O:24]1.C(N(CC)CC)C>C1C=CC=CC=1>[CH3:1][O:2][C:3]1[C:8]([O:9][CH2:10][O:11][CH3:12])=[CH:7][C:6]([O:13][CH3:14])=[C:5]([O:15][CH2:16][O:17][CH3:18])[C:4]=1[CH2:19][CH:20]=[C:27]1[C:28](=[O:29])[O:30][C:23]([CH3:31])([CH3:22])[O:24][C:25]1=[O:26]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 162492,2-Dimethyl-1,3-dioxane-4,6-dioneHCID 197572302-[2,5-Dimethoxy-3,6-bis(methoxymethoxy)phenyl]acetoaldehyde

生成物 1

HCID 197571651-[2,5-Dimethoxy-3,6-bis(methoxymethoxy)phenyl]-2-(2,2-dimethyl-4,6-dioxo-1,3-dioxan-5-ylidene)ethane

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

実験手順

2.7 Grams (9.0 mM) of 2-[2,5-dimethoxy-3,6-bis(methoxymethoxy)phenyl]acetoaldehyde was dissolved in 80 ml of benzene, then to this solution was added 1.56 g (10.8 mM) of Meldrum's acid (2,2-dimethyl-1,3-dioxane-4,6-dione) and 2.18 g (21.6 mM) of triethylamine were added and the reaction mixture was stirred at room temperature for 12 hours. 100 Milliliters of benzene was added to the reaction mixture and washed twice with 200 ml of water and further washed twice with a saturated sodium chloride aqueous solution, then the benzene solution was dried over anhydrous magnesium sulfate. The benzene solution was concentrated under reduced pressure and the residue obtained was purified by a silica gel column chromatography (diameter 5 cm×length 15 cm, eluent: 30% ethyl acetatehexane, "Wakogel C-200") to yield 2.9 g of 1-[2,5-dimethoxy-3,6-bis(methoxymethoxy)phenyl]-2-(2,2-dimethyl-4,6-dioxo-1,3-dioxan-5-ylidene)ethane. Light yellow indefinite form powdery substance.

後処理

  1. additionwere added
  2. washwashed twice with 200 ml of water
  3. washfurther washed twice with a saturated sodium chloride aqueous solution
  4. dry with materialthe benzene solution was dried over anhydrous magnesium sulfate
  5. concentrationThe benzene solution was concentrated under reduced pressure
  6. customthe residue obtained
  7. customwas purified by a silica gel column chromatography (diameter 5 cm×length 15 cm, eluent: 30% ethyl acetatehexane, "Wakogel C-200")

出典と根拠

ORDレコード
ord-7ed268b4d2c64e95bd58f109c77cbf37
出典データセット
uspto-grants-1993_06
特許番号
US05220042

反応ノート

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