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Pyridine → HCID 86597335、化合物

HRID 2182193
ノート
印刷プレビュー

反応式

HRID 2182193 の反応式
[F:1][C:2]([F:16])([C:6]([F:15])([F:14])[C:7]([F:13])([F:12])[C:8]([F:11])([F:10])[F:9])[CH2:3][CH2:4][OH:5].N1C=CC=CC=1.C(N(CC)CC)C.[Cl-].[C:31]([O:38][CH2:39][CH:40]([CH2:45][CH3:46])[CH2:41][CH2:42][CH2:43][CH3:44])(=[O:37])/[CH:32]=[CH:33]\[C:34]([O-])=[O:35]>C(Cl)(Cl)Cl>[C:31]([O:38][CH2:39][CH:40]([CH2:45][CH3:46])[CH2:41][CH2:42][CH2:43][CH3:44])(=[O:37])/[CH:32]=[CH:33]\[C:34]([O:5][CH2:4][CH2:3][C:2]([F:16])([F:1])[C:6]([F:14])([F:15])[C:7]([F:12])([F:13])[C:8]([F:9])([F:10])[F:11])=[O:35]
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 4

HCID 1049PyridineHCID 8471TriethylamineHCID 748831-Hexanol, 3,3,4,4,5,5,6,6,6-nonafluoro-HCID 86590608HCID 86590608、化合物

生成物 1

HCID 86597335HCID 86597335、化合物収率 54.9%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

3,3,4,4,5,5,6,6,6-Nonafluorohexanol (515 g, 1.95 mol), pyridine (169 g, 2.13 mol) and triethylamine (394 mL, 3.89 mol) were dissolved in chloroform (1000 mL) and added dropwise with 2-ethylhexyl maleate chloride (530 g, 2.14 mol), while the internal temperature was kept at 20° C. or lower on an ice bath. After completion of the addition, the reaction mixture was stirred at room temperature for 1 hour and then added with chloroform. The organic phase was washed with water and a saturated sodium chloride aqueous solution. Then, the organic layer was collected, and the organic solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/chloroform=10/0 to 7/3 (v/v)) to obtain the target compound (508 g, yield: 50%), which was colorless and transparent.

後処理

  1. customwas kept at 20° C. or lower on an ice bath
  2. additionAfter completion of the addition
  3. washThe organic phase was washed with water
  4. customThen, the organic layer was collected
  5. customthe organic solvent was evaporated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (hexane/chloroform=10/0 to 7/3 (v/v))

出典と根拠

ORDレコード
ord-654e3e77056f4150a3da9dd3f3d9a81c
出典データセット
uspto-grants-2005_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06897013B2

反応ノート

読み込み中…

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