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Water → (-)-2-(4-(4-Octyloxy-5,5,5-trifluoro-1-pentyl)phenyl)-5-decyloxypyrimidine

HRID 1735983
ノート
印刷プレビュー

反応式

HRID 1735983 の反応式
[OH:1][CH:2]([C:29]([F:32])([F:31])[F:30])[CH2:3][CH2:4][CH2:5][C:6]1[CH:11]=[CH:10][C:9]([C:12]2[N:17]=[CH:16][C:15]([O:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])=[CH:14][N:13]=2)=[CH:8][CH:7]=1.[H-].[K+].C1(C)C=CC(S(O[CH2:45][CH2:46][CH2:47][CH2:48][CH2:49][CH2:50][CH2:51][CH3:52])(=O)=O)=CC=1.O>O1CCCC1.C1(C)C=CC=CC=1>[CH2:45]([O:1][CH:2]([C:29]([F:31])([F:32])[F:30])[CH2:3][CH2:4][CH2:5][C:6]1[CH:7]=[CH:8][C:9]([C:12]2[N:17]=[CH:16][C:15]([O:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])=[CH:14][N:13]=2)=[CH:10][CH:11]=1)[CH2:46][CH2:47][CH2:48][CH2:49][CH2:50][CH2:51][CH3:52]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 82127Potassium hydrideHCID 599296n-Octyl p-ToluenesulfonateHCID 19694914(-)-2-(4-(4-Hydroxy-5,5,5-trifluoro-1-pentyl)phenyl)-5-decyloxypyrimidine

生成物 1

HCID 19435043(-)-2-(4-(4-Octyloxy-5,5,5-trifluoro-1-pentyl)phenyl)-5-decyloxypyrimidine収率 56.7%

試薬・触媒・溶媒 2

HCID 1140
Toluene
溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

1.1 g (2.5 mmol) of (-)-2-(4-(4-hydroxy-5,5,5-trifluoro-1-pentyl)phenyl)-5-decyloxypyrimidine was dissolved in 10 ml of tetrahydrofuran. This solution was added with 0.12 g (3 mmol) of potassium hydride, stirred at 10°-20° C. for 20 minutes, further added with 0.85 g (3 mmol) of octyl p-toluenesulfonate and reacted at 20°-30° C. for 2 hours. The reaction mixture was poured into 100 ml of water and 100 ml of toluene, and the toluene layer was washed with water and concentrated under reduced pressure. The residue was purified by silica gel column chromatography using toluene/ethyl acetate as eluent to obtain 0.80 g of (-)-2-(4-(4-octyloxy-5,5,5-trifluoro-1-pentyl)phenyl)-5-decyloxypyrimidine

後処理

  1. customreacted at 20°-30° C. for 2 hours
  2. washthe toluene layer was washed with water
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-1789afb5355746d8aebc00d8001c9cc7
出典データセット
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05539115

反応ノート

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