Chlorosulfonic acid → Ethyl 2-(4-(chlorosulfonyl)-2-ethylphenoxy)acetate

HRID 1766115

반응식

HRID 1766115 반응식
[CH2:1]([C:3]1[CH:15]=[CH:14][CH:13]=[CH:12][C:4]=1[O:5][CH2:6][C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH3:2].[Cl:16][S:17](O)(=[O:19])=[O:18]>>[Cl:16][S:17]([C:14]1[CH:13]=[CH:12][C:4]([O:5][CH2:6][C:7]([O:9][CH2:10][CH3:11])=[O:8])=[C:3]([CH2:1][CH3:2])[CH:15]=1)(=[O:19])=[O:18]

참가 물질

3

반응물 2

HCID 24638Chlorosulfonic acidHCID 21986411Ethyl (2-ethylphenoxy)acetate

생성물 1

HCID 21986343Ethyl 2-(4-(chlorosulfonyl)-2-ethylphenoxy)acetate수율 70%

반응 조건

온도
0 °C

실험 절차

To a 250 ml round-bottom flask containing chlorosulfonic acid (30 ml) cooled to 0° C. was added ethyl (2-ethylphenoxy)acetate (7.2 g, 34.6 mmoles) dropwise. Once the addition was complete the ice-bath was removed and the reaction was allowed to warm to room temperature at which the reaction was stirred for 3 hours. The reaction was then slowly added to ice and, once the excess chlorosulfonic acid was quenched, the mixture was diluted with CH2Cl2 (200 ml). The phases were separated and the aqueous fraction was washed with CH2Cl2 twice. The combined organic fractions were dried over Na2SO4 and filtered and concentrated in vacuo to yield 7.2 g (70%) of crude product. The crude product was used with no purification.

후처리

  1. additionOnce the addition
  2. customwas removed
  3. temperatureto warm to room temperature at which the reaction
  4. additionThe reaction was then slowly added to ice
  5. customonce the excess chlorosulfonic acid was quenched
  6. additionthe mixture was diluted with CH2Cl2 (200 ml)
  7. customThe phases were separated
  8. washthe aqueous fraction was washed with CH2Cl2 twice
  9. dry with materialThe combined organic fractions were dried over Na2SO4
  10. filtrationfiltered
  11. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-2e0e51a231b6470393197a0a42a9a039
출처 데이터셋
uspto-grants-2007_06
특허 번호
US07229998B2

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