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Acetyl chloride → HCID 19600991, 화합물

HRID 610078
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HRID 610078 반응식
[F:1][C:2]([F:15])([F:14])[CH2:3][N:4]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH2:6][C:5]1=[O:13].[C:16](Cl)(=[O:18])[CH3:17].[Cl-].[Cl-].[Cl-].[Al+3]>C(=S)=S>[C:16]([C:9]1[CH:8]=[C:7]2[C:12](=[CH:11][CH:10]=1)[N:4]([CH2:3][C:2]([F:1])([F:14])[F:15])[C:5](=[O:13])[CH2:6]2)(=[O:18])[CH3:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6367Acetyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 196009761-(2,2,2-Trifluoro-ethyl)-1,3-dihydro-indol-2-one

생성물 1

HCID 19600991HCID 19600991, 화합물

시약·촉매·용매 1

HCID 6348Carbon Disulfide용매

실험 절차

To a solution of 1-(2,2,2-trifluoro-ethyl)-1,3-dihydro-indol-2-one (2.0 g, 9.3 mmol) and acetyl chloride (0.86 mL, 12 mmol) in carbon disulfide (40 mL) was added aluminum trichloride (7.4 g, 56 mmol) by portions. The mixture was heated to reflux for 3 hours, then cooled. The liquid phase was decanted and the residue was quenched carefully with ice, then water. The solids were filtered, washed with water, dried and recrystallized from acetone/hexanes to give a pale pink solid, mp 170-171° C. Yield 1.23 g (51%).

후처리

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 3 hours
  3. temperaturecooled
  4. customThe liquid phase was decanted
  5. customthe residue was quenched carefully with ice
  6. filtrationThe solids were filtered
  7. washwashed with water
  8. customdried
  9. customrecrystallized from acetone/hexanes
  10. customto give a pale pink solid, mp 170-171° C

출처 및 근거

ORD 기록
ord-5c6b02960a8a422ca3d010efc9cecdb6
출처 데이터셋
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05998463

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