ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

4-Iodobenzaldehyde → HCID 72326541、化合物

HRID 1176970
ノート
印刷プレビュー

反応式

HRID 1176970 の反応式
[CH2:1]([O:13][C:14]1[CH:15]=[C:16]([CH:33]2[S:38][CH2:37][CH2:36][CH2:35][S:34]2)[CH:17]=[CH:18][C:19]=1[O:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].[Li]CCCC.[I:44][C:45]1[CH:52]=[CH:51][C:48]([CH:49]=[O:50])=[CH:47][CH:46]=1>C1COCC1>[CH2:1]([O:13][C:14]1[CH:15]=[C:16]([C:33]2([CH:49]([C:48]3[CH:51]=[CH:52][C:45]([I:44])=[CH:46][CH:47]=3)[OH:50])[S:34][CH2:35][CH2:36][CH2:37][S:38]2)[CH:17]=[CH:18][C:19]=1[O:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 966574-IodobenzaldehydeHCID 59560834HCID 59560834、化合物HCID 178418339Butyllithium

生成物 1

HCID 72326541HCID 72326541、化合物収率 65.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

A solution of 2-(3,4-bis-dodecyloxy-phenyl)-[1,3]dithiane (12.0 g, 21.1 mmol) in 120 mL of dry THF in a Schlenk tube was cooled down to −78° C. Under N2 atmosphere, n-BuLi (9.4 mL of 2.5 M solution in hexanes, 23.4 mmol) was added dropwise to the mixture. After stirring at 0° C. for 1 h, the reaction mixture was cooled down to −78° C. and 4-iodobenzaldehyde (3.72 g, 16.0 mmol) in 100 mL of dry THF was added dropwise. The resulting mixture was allowed to warm up to room temperature and stirred at room temperature overnight. The reaction was quenched with H2O and THF was removed under reduced pressure. The resulting slurry was extracted with CH2Cl2 and the organic layer was washed with H2O and dried over anhydrous MgSO4. The solvent was removed under reduced pressure. The product was purified by column chromatography (silica gel, hexanes:dichloromethane=3:2, 1:1, then 2:3 (v/v)) to give light yellow oil (8.3 g, 65%). 1H NMR (300 MHz, CDCl3, δ): 7.44 (d, J=8.2 Hz, 2H), 7.23 (dd, J=8.5 Hz, 2.5 Hz, 1H), 7.02 (d, J=2.5 Hz, 1H), 6.78 (d, J=8.5 Hz, 1H), 6.61 (d, J=8.5 Hz, 2H), 4.84 (s, 1H), 3.98 (t, J=6.6 Hz, 2H), 3.73 (m, 2H), 3.00 (s, 1H), 2.69 (m, 4H), 1.66-1.94 (m, 6H), 1.20-1.51 (m, 36H), 0.86 (t, J=6.7 Hz, 6H). 13C{1H} NMR (75 MHz, CDCl3, δ): 148.40, 148.31, 136.96, 135.88, 130.04, 128.93, 122.95, 115.99, 112.55, 93.82, 80.51, 69.29, 69.05, 66.33, 32.00, 29.78, 29.72, 29.55, 29.45, 29.32, 29.29, 27.41, 27.02, 26.12, 24.80, 22.78, 14.24. LRMS-EI (m/z): [M−H2O]+ calcd for C41H63IO2S2, 778.3; found, 778.5.

後処理

  1. temperaturethe reaction mixture was cooled down to −78° C.
  2. temperatureto warm up to room temperature
  3. stirringstirred at room temperature overnight
  4. customThe reaction was quenched with H2O and THF
  5. customwas removed under reduced pressure
  6. extractionThe resulting slurry was extracted with CH2Cl2
  7. washthe organic layer was washed with H2O
  8. dry with materialdried over anhydrous MgSO4
  9. customThe solvent was removed under reduced pressure
  10. customThe product was purified by column chromatography (silica gel, hexanes

出典と根拠

ORDレコード
ord-c57528c267bf4b08b0a50e5d836c7f59
出典データセット
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07842830B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート