Hydrochloric Acid → 3,3',5,5'-Tetramethyl-7,7'-bis(3,5-diethynylphenyl)-1,1'-biadamantane

HRID 39118ノート

反応式

HRID 39118 の反応式
[CH3:1][C:2]12[CH2:12][C:6]3([C:13]4[CH:18]=[C:17]([C:19]#[C:20][Si](C)(C)C)[CH:16]=[C:15]([C:25]#[C:26][Si](C)(C)C)[CH:14]=4)[CH2:7][C:8]([CH3:11])([CH2:10][C:4]([C:31]45[CH2:58][C:35]6([CH3:59])[CH2:36][C:37]([C:40]7[CH:45]=[C:44]([C:46]#[C:47][Si](C)(C)C)[CH:43]=[C:42]([C:52]#[C:53][Si](C)(C)C)[CH:41]=7)([CH2:39][C:33]([CH3:60])([CH2:34]6)[CH2:32]4)[CH2:38]5)([CH2:5]3)[CH2:3]1)[CH2:9]2.C(=O)([O-])[O-].[K+].[K+].O1CCCC1.Cl>CO>[CH3:60][C:33]12[CH2:39][C:37]3([C:40]4[CH:45]=[C:44]([C:46]#[CH:47])[CH:43]=[C:42]([C:52]#[CH:53])[CH:41]=4)[CH2:36][C:35]([CH3:59])([CH2:58][C:31]([C:4]45[CH2:10][C:8]6([CH3:11])[CH2:7][C:6]([C:13]7[CH:18]=[C:17]([C:19]#[CH:20])[CH:16]=[C:15]([C:25]#[CH:26])[CH:14]=7)([CH2:12][C:2]([CH3:1])([CH2:9]6)[CH2:3]4)[CH2:5]5)([CH2:38]3)[CH2:32]1)[CH2:34]2

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 11430Potassium CarbonateHCID 575583753,3',5,5'-Tetramethyl-7,7'-bis[3,5-bis(trimethylsilylethynyl)phenyl]-1,1'-biadamantane

生成物 1

HCID 575583763,3',5,5'-Tetramethyl-7,7'-bis(3,5-diethynylphenyl)-1,1'-biadamantane

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Next, 39.8 g (53.5 mmol) of the previously obtained 3,3′,5,5′-tetramethyl-7,7′-bis[3,5-bis(trimethylsilylethynyl)phenyl]-1,1′-biadamantane and 1.46 g (10.6 mmol) of potassium carbonate were stirred in a mixed solvent comprising 600 ml of tetrahydrofuran and 300 ml of methanol, for 4 hours under a nitrogen atmosphere at room temperature. This was added to 1000 ml of a 10% hydrochloric acid aqueous solution, and the precipitate was filtered and washed with 1000 ml of water and then with 1000 ml of acetone, after which it was dried to obtain 21.2 g of 3,3′,5,5′-tetramethyl-7,7′-bis(3,5-diethynylphenyl)-1,1′-biadamantane.

後処理

  1. filtrationthe precipitate was filtered
  2. washwashed with 1000 ml of water
  3. dry with materialwith 1000 ml of acetone, after which it was dried

出典と根拠

ORDレコード
ord-3190d20bc4634203ba9fb38fff4a2f38
出典データセット
uspto-grants-2013_09
特許番号
US08524847B2

反応ノート

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