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Ammonium Hydroxide → (E)-2-(6-fluoro-1-indanylidene)acetamide

HRID 362813
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HRID 362813 반응식
[OH-].[NH4+:2].[F:3][C:4]1[CH:12]=[C:11]2[C:7]([CH2:8][CH2:9]/[C:10]/2=[CH:13]\[C:14](Cl)=[O:15])=[CH:6][CH:5]=1>ClCCl>[F:3][C:4]1[CH:12]=[C:11]2[C:7]([CH2:8][CH2:9]/[C:10]/2=[CH:13]\[C:14]([NH2:2])=[O:15])=[CH:6][CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14923Ammonium HydroxideHCID 15491026(E)-2-(6-fluoro-1-indanylidene)acetyl chloride

생성물 1

HCID 9837001(E)-2-(6-fluoro-1-indanylidene)acetamide수율 91%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A 29.6% aqueous ammonium hydroxide solution (17.6 mL, 134 mmol) was added dropwise to a stirred, chilled (ice bath) solution of (E)-2-(6-fluoro-1-indanylidene)acetyl chloride (14.1 g, 67 mmol) in dichloromethane (165 mL). After an hour, the resulting white precipitate was collected by filtration, dissolved in ethyl acetate (600 mL) and washed with water (3×300 mL). The ethyl acetate layer was dried over sodium sulfate and concentrated in vacuo. The resulting off-white solid was washed with hexane, giving 11.6 g (91%) of (E)-2-(6-fluoro-1-indanylidene)acetamide, m.p., 180°-183° C.;

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후처리

  1. waitAfter an hour
  2. filtrationthe resulting white precipitate was collected by filtration
  3. dissolutiondissolved in ethyl acetate (600 mL)
  4. washwashed with water (3×300 mL)
  5. dry with materialThe ethyl acetate layer was dried over sodium sulfate
  6. concentrationconcentrated in vacuo
  7. washThe resulting off-white solid was washed with hexane

출처 및 근거

ORD 기록
ord-e85e9a9eea4840ed80529731996f7760
출처 데이터셋
uspto-grants-1999_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05872118

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