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Chlorosulfonic acid → HCID 12838042, 화합물

HRID 1447112
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HRID 1447112 반응식
[C:1]([N:4]1[CH2:13][CH2:12][C:11]2[C:6](=[CH:7][C:8]([Cl:14])=[CH:9][CH:10]=2)[CH2:5]1)(=[O:3])[CH3:2].[Cl:15][S:16](O)(=[O:18])=[O:17]>C(Cl)(Cl)Cl>[C:1]([N:4]1[CH2:13][CH2:12][C:11]2[C:6](=[CH:7][C:8]([Cl:14])=[C:9]([S:16]([Cl:15])(=[O:18])=[O:17])[CH:10]=2)[CH2:5]1)(=[O:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24638Chlorosulfonic acidHCID 12838039HCID 12838039, 화합물

생성물 1

HCID 12838042HCID 12838042, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

A solution of 2.0 g. (0.01 mole) 2-acetyl-7-chloro-1,2,3,4-tetrahydroisoquinoline in 15 ml. dry chloroform is added dropwise to 20 ml. chlorosulfonic acid at ambient temperature. The reaction mixture is stirred at ambient temperature for 24 hours and then refluxed at 60° C. for 2 hours. The reaction mixture is then cooled, poured onto a liter of ice and extracted with methylene chloride. The organic phase is dried over anhydrous magnesium sulfate, filtered and the filtrate is concentrated to dryness under reduced pressure to yield the desired product.

후처리

  1. customat ambient temperature
  2. temperaturerefluxed at 60° C. for 2 hours
  3. temperatureThe reaction mixture is then cooled
  4. extractionextracted with methylene chloride
  5. dry with materialThe organic phase is dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationthe filtrate is concentrated to dryness under reduced pressure

출처 및 근거

ORD 기록
ord-4dbc6d6f80324560a5ffd66c2cfcd079
출처 데이터셋
uspto-grants-1982_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04315935

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