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Isatin → HCID 19600971, 화합물

HRID 610076
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HRID 610076 반응식
[NH:1]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:4](=[O:5])[C:2]1=[O:3].[F:12][C:13]([F:17])([F:16])[CH2:14]I>O>[F:12][C:13]([F:17])([F:16])[CH2:14][N:1]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:4](=[O:5])[C:2]1=[O:3]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 7054IsatinHCID 677091,1,1-Trifluoro-2-iodoethane

생성물 1

HCID 19600971HCID 19600971, 화합물

시약·촉매·용매 1

HCID 962Water용매

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온도
55 °C

실험 절차

Sodium hydride (8.65 g of a 60% oil dispersion, 0.22 mol) was washed with hexane and suspended in hexamethylphosphoramide (200 mL). Isatin (29.4 g, 0.20 mol)) was added carefully. After the gas evolution subsided, 2,2,2-trifluoroethyl iodide (46.2 g, 0.22 mol) was added and the mixture was heated to 55° C. for 4 hours. The solution was cooled, diluted with water (1 L), and the precipitate was collected. The filtrate was acidified with 6 N HCl and a new precipitate formed and was collected. The combined solids were recrystallized from 95% ethanol. Yield 22.5 g (49%). mp 161-163° C.

후처리

  1. washSodium hydride (8.65 g of a 60% oil dispersion, 0.22 mol) was washed with hexane
  2. temperatureThe solution was cooled
  3. customthe precipitate was collected
  4. customa new precipitate formed
  5. customwas collected
  6. customThe combined solids were recrystallized from 95% ethanol

출처 및 근거

ORD 기록
ord-75715625ac8c4c20a15efd9d6974e6d7
출처 데이터셋
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05998463

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