Potassium Carbonate → Methyl 5-[(3-iodo-5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalen-2-yloxy)-acetyl]-3-thiophenecarboxylate

HRID 1075625

反応式

HRID 1075625 の反応式
[I:1][C:2]1[C:3]([OH:16])=[CH:4][C:5]2[C:6]([CH3:15])([CH3:14])[CH2:7][CH2:8][C:9]([CH3:13])([CH3:12])[C:10]=2[CH:11]=1.Br[CH2:18][C:19]([C:21]1[S:25][CH:24]=[C:23]([C:26]([O:28][CH3:29])=[O:27])[CH:22]=1)=[O:20].C(=O)([O-])[O-].[K+].[K+]>C(C(C)=O)C>[I:1][C:2]1[C:3]([O:16][CH2:18][C:19]([C:21]2[S:25][CH:24]=[C:23]([C:26]([O:28][CH3:29])=[O:27])[CH:22]=2)=[O:20])=[CH:4][C:5]2[C:6]([CH3:15])([CH3:14])[CH2:7][CH2:8][C:9]([CH3:12])([CH3:13])[C:10]=2[CH:11]=1

参加物

5

実験手順

A solution of 3-iodo-5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalen-2-ol (4 g, 12.1 mmol), methyl 5-bromoacetyl-3-thiophenecarboxylate (3.18 g, 12.1 mmol) and potassium carbonate (1.84 g, 13.3 mmol) in methyl ethyl ketone (100 ml), was heated under reflux for 4 h. The reaction medium was filtered and then concentrated in a rotary evaporator. The mixture was extracted with ethyl ether. The organic phase was washed with water, dried over magnesium sulfate and concentrated in a rotary evaporator under vacuum at 40° C.

後処理

  1. temperatureunder reflux for 4 h
  2. filtrationThe reaction medium was filtered
  3. concentrationconcentrated in a rotary evaporator
  4. extractionThe mixture was extracted with ethyl ether
  5. washThe organic phase was washed with water
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated in a rotary evaporator under vacuum at 40° C.

出典と根拠

ORDレコード
ord-f15a7a82bcb745ee9e03b7f2f77866b9
出典データセット
uspto-grants-1999_05
特許番号
US05905088

関連ノート

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