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

HRID 39118노트

반응식

HRID 39118 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3190d20bc4634203ba9fb38fff4a2f38
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08524847B2

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