Chlorosulfonic acid → HCID 18541162, 화합물

HRID 411603노트

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HRID 411603 반응식
[O:1]([CH2:8][CH2:9][N:10]1[CH2:15][CH2:14][O:13][CH2:12][CH2:11]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.O(CCN1CCOCC1)C1C=CC=CC=1.[Cl:32][S:33](O)(=[O:35])=[O:34]>ClCCl>[N:10]1([CH2:9][CH2:8][O:1][C:2]2[CH:7]=[CH:6][C:5]([S:33]([Cl:32])(=[O:35])=[O:34])=[CH:4][CH:3]=2)[CH2:11][CH2:12][O:13][CH2:14][CH2:15]1

참가 물질

5

반응물 3

HCID 24638Chlorosulfonic acid2회HCID 28409994-(2-Phenoxyethyl)morpholineHCID 6996069929488-54-8

생성물 1

HCID 18541162HCID 18541162, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
0 °C

실험 절차

[2-(Morpholin-4-yl)ethoxy]benzene-4-sulfonyl chloride was prepared using N-(2-phenoxyethyl) morpholine by similar reaction described above. For example, 7.2 g of N-(2-phenoxyethyl)morpholine HCl salt was resuspended in 20 ml of dichloromethane and 7 ml of chlorosulfonic acid was slowly introduced with cooling by ice-jacket. The reaction mixture was stirred at 0° C. for 2 hr, then, at room temperature overnight. Dichloromethane (350 ml) was added to the reaction mixture and excess chlorosulfonic acid was destroyed by adding icy water(about 100 g). Aqueous layer was adjusted to pH 8.5 by concentrated sodium carbonate solution with cooling by ice. Dichloromethane was dried over anhydrous magnesium sulfate and evaporated under reduced pressure to give 8.1 g of [2-(morpholin-4-yl)ethoxy]benzene-4-sulfonyl chloride. M.P. 48-50° C.

후처리

  1. custom[2-(Morpholin-4-yl)ethoxy]benzene-4-sulfonyl chloride was prepared
  2. customby similar reaction
  3. temperaturewith cooling by ice-jacket
  4. customat room temperature
  5. customovernight
  6. customwas destroyed
  7. additionby adding icy water(about 100 g)
  8. temperaturewith cooling by ice
  9. dry with materialDichloromethane was dried over anhydrous magnesium sulfate
  10. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-dbb985ddc5d043828975100e1d40228c
출처 데이터셋
uspto-grants-2003_05
특허 번호
US06559167B1

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