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Pyridine → HCID 86597335, 화합물

HRID 2182193
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HRID 2182193 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 1049PyridineHCID 8471TriethylamineHCID 748831-Hexanol, 3,3,4,4,5,5,6,6,6-nonafluoro-HCID 86590608HCID 86590608, 화합물

생성물 1

HCID 86597335HCID 86597335, 화합물수율 54.9%

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

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.

후처리

  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))

출처 및 근거

ORD 기록
ord-654e3e77056f4150a3da9dd3f3d9a81c
출처 데이터셋
uspto-grants-2005_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06897013B2

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