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Diethyl Ether → HCID 14439127、化合物

HRID 1849948
ノート
印刷プレビュー

反応式

HRID 1849948 の反応式
[CH2:1]([C:11]1[CH:12]=[N:13][C:14]([C:17]2[CH:22]=[CH:21][C:20](O)=[CH:19][CH:18]=2)=[N:15][CH:16]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10].[C:24]([O-:27])([O-])=O.[Cs+].[Cs+].CCO[CH2:33][CH3:34]>CN(C)C=O>[CH2:1]([C:11]1[CH:12]=[N:13][C:14]([C:17]2[CH:22]=[CH:21][C:20]([O:27][CH2:24][CH2:11][CH2:1][CH2:2][CH2:3][CH:33]=[CH2:34])=[CH:19][CH:18]=2)=[N:15][CH:16]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10].[CH2:1]([C:11]1[CH:12]=[N:13][C:14]([C:17]2[CH:22]=[CH:21][C:20]([O:27][CH2:24][CH2:3][CH2:2][CH2:1][CH2:11][CH2:16][CH:33]=[CH2:34])=[CH:19][CH:18]=2)=[N:15][CH:16]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10]
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 3

HCID 3283Diethyl EtherHCID 10796Cesium carbonateHCID 135585902Phenol, 4-(5-decyl-2-pyrimidinyl)-

生成物 2

HCID 14439127HCID 14439127、化合物HCID 198347485-Decyl-2-(4-(hept-6-enyloxy)phenyl)pyrimidine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Vinyl-terminated phenyl pyrimidines with different spacer lengths were synthesized from 4-(5-decylpyrimidin-2-yl)phenol for siloxane coupling to 1,2 polybutadiene. A general procedure for this synthesis is as follows: 4-(5-decylpyrimidin-2-yl)phenol (1.89 grams, 6.05 mmols), a bromoalkene (7-bromo hept-1-ene, 8-bromooct-1-ene or 10-bromododec-1-ene, 8 mmol) and Cs2CO3 (2.56 grams, 8 mmols) were stirred at room temperature in 40 mL of dimethyl formamide overnight, resulting in near-quantitative conversion to the ether (Scheme 3), monitored by thin layer chromatography. The reaction mixture was extracted three times with 50 mL of dichloromethane. The organic extracts were washed three times with water and dried with MgSO4. The crude product was recrystallized in hot 95% ethanol, resulting in analytically pure white crystals of 5-decyl-2-(4-(hept-6-enyloxy)phenyl)pyrimidine, 5-decyl-2-(4-(oct-7-enyloxy)phenyl)pyrimidine, -decyl-2-(4-(dec-9-enyloxy)phenyl)pyrimidine (1.20 g, 2.09 g, 1.69 g AND 48.0%, 83.6%, 66.02% overall yield, respectively).

後処理

  1. customVinyl-terminated phenyl pyrimidines with different spacer lengths
  2. customwere synthesized from 4-(5-decylpyrimidin-2-yl)phenol for siloxane coupling to 1,2 polybutadiene
  3. extractionThe reaction mixture was extracted three times with 50 mL of dichloromethane
  4. washThe organic extracts were washed three times with water
  5. dry with materialdried with MgSO4
  6. customThe crude product was recrystallized in hot 95% ethanol

出典と根拠

ORDレコード
ord-39560a42cee9448f8d9d228d3cfc61ff
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08956705B2

反応ノート

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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