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Potassium Carbonate → HCID 67780109、化合物

HRID 1648015
ノート
印刷プレビュー

反応式

HRID 1648015 の反応式
[CH3:1][O:2][C:3](=[O:23])/[CH:4]=[CH:5]/[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[O:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][O:18]S(C)(=O)=O.[O:24]=[C:25]1[CH2:34][CH2:33][CH2:32][C:31]2[C:30](O)=[C:29]([CH2:36][CH:37]=[CH2:38])[CH:28]=[CH:27][C:26]1=2.C(=O)([O-])[O-].[K+].[K+].COCCOCCN(CCOCCOC)CCOCCOC>CCOCC.C1(C)C=CC=CC=1>[CH3:1][O:2][C:3](=[O:23])/[CH:4]=[CH:5]/[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[O:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][O:18][C:30]1[C:31]2[CH2:32][CH2:33][CH2:34][C:25](=[O:24])[C:26]=2[CH:27]=[CH:28][C:29]=1[CH2:36][CH:37]=[CH2:38]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 11430Potassium Carbonate2 回HCID 112414Ethanamine, 2-(2-methoxyethoxy)-N,N-bis[2-(2-methoxyethoxy)ethyl]-HCID 199221065-Oxo-2-(2-propenyl)-5,6,7,8-tetrahydro-1-naphthalenolHCID 86747453HCID 86747453、化合物

生成物 1

HCID 67780109HCID 67780109、化合物収率 96%

試薬・触媒・溶媒 2

HCID 1140
Toluene
溶媒
HCID 3283Diethyl Ether溶媒

実験手順

A mixture of 1.37 g (4 mmol) of (E)-3-[2-[[5-[(methylsulfonyl)oxy]pentyl]oxy]phenyl]-2-propenoic acid methyl ester from example 76, 0.81 g (4 mmol) of 5-oxo-2-(2-propenyl)-5,6,7,8-tetrahydro-1-naphthalenol, 0.8 g (5.8 mmol) of anhydrous, granular potassium carbonate, 0.08 mL of TDA-1, and 25 mL of toluene was stirred under reflux for 5.5 hr and at room temperature for 12 hr. After being treated with 0.3 g of additional potassium carbonate, the mixture was stirred and refluxed for a further 24 hr. The mixture was cooled and diluted with ether. The organic phase was washed with water and saturated brine and work-up was completed in the usual manner giving a brown oil. This material was chomatographed on 50 g of silica gel. Elution with 1:1 hexane-ether afforded 1.72 g (96%) of (E)-3-[2-[5-[(5-oxo-2-(2-propenyl)- 5,6,7,8-tetrahydro-1-naphthalenyl)oxy]pentyloxy]phenyl]-2-propenoic acid methyl ester as a yellow-orange oil.

後処理

  1. stirringthe mixture was stirred
  2. temperaturerefluxed for a further 24 hr
  3. temperatureThe mixture was cooled
  4. washThe organic phase was washed with water and saturated brine
  5. customgiving a brown oil
  6. washElution with 1:1 hexane-ether

出典と根拠

ORDレコード
ord-f106494851f4420b9afb4e9349e7eaf7
出典データセット
uspto-grants-1995_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05434186

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート