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Triethylamine → 2-(1,2,3,4-tetramethoxy-6,7,8,9-tetrahydro-5H-benzo[a]cyclohepten-7-yl)ethyl methanesulfonate

HRID 2268493
ノート
印刷プレビュー

反応式

HRID 2268493 の反応式
[CH3:1][O:2][C:3]1[C:8]2[CH2:9][CH2:10][CH:11]([CH2:14][CH2:15][OH:16])[CH2:12][CH2:13][C:7]=2[C:6]([O:17][CH3:18])=[C:5]([O:19][CH3:20])[C:4]=1[O:21][CH3:22].C(N(CC)CC)C.[CH3:30][S:31](Cl)(=[O:33])=[O:32].C(=O)(O)[O-].[Na+]>C(#N)C>[CH3:30][S:31]([O:16][CH2:15][CH2:14][CH:11]1[CH2:12][CH2:13][C:7]2[C:6]([O:17][CH3:18])=[C:5]([O:19][CH3:20])[C:4]([O:21][CH3:22])=[C:3]([O:2][CH3:1])[C:8]=2[CH2:9][CH2:10]1)(=[O:33])=[O:32]
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 4

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 516892Sodium BicarbonateHCID 183486172-(1,2,3,4-Tetramethoxy-6,7,8,9-tetrahydro-5H-benzo[a]cyclohepten-7-yl)ethanol

生成物 1

HCID 183485372-(1,2,3,4-tetramethoxy-6,7,8,9-tetrahydro-5H-benzo[a]cyclohepten-7-yl)ethyl methanesulfonate

試薬・触媒・溶媒 1

HCID 6342
Acetonitrile
溶媒

実験手順

To a solution of 2-(1,2,3,4-tetramethoxy-6,7,8,9-tetrahydro-5H-benzo[a]cyclohepten-7-yl)ethanol (2.50 g) and triethylamine (1.68 ml) in acetonitrile (50 ml) was dropwise added methanesufonyl chloride (0.750 ml) with cooling with ice. After the reaction mixture was stirred for 15 min, saturated aqueous sodium bicarbonate was added to the solution with cooling with ice, which was extracted with ethyl acetate. The organic layer was washed with 1N hydrochloric acid, water, saturated aqueous sodium bicarbonate, water, and saturated aqueous sodium chloride, and dried. The solvent was removed in vacuo to yield the entitled compound (3.12 g) as an oil.

後処理

  1. temperaturewith cooling with ice
  2. temperaturewith cooling with ice, which
  3. extractionwas extracted with ethyl acetate
  4. washThe organic layer was washed with 1N hydrochloric acid, water, saturated aqueous sodium bicarbonate, water, and saturated aqueous sodium chloride
  5. customdried
  6. customThe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-5131699bce744640abc1975772b825f3
出典データセット
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06326369B1

反応ノート

読み込み中…

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