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Triethylamine → HCID 5181860, 화합물

HRID 1643467
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HRID 1643467 반응식
[F:1][C:2]([F:14])([F:13])[C:3]1[CH:4]=[C:5]([S:9](Cl)(=[O:11])=[O:10])[CH:6]=[CH:7][CH:8]=1.[NH:15]1[CH2:20][CH2:19][CH2:18][CH2:17][CH:16]1[CH2:21][OH:22].C(N(CC)CC)C>C(Cl)Cl>[F:1][C:2]([F:14])([F:13])[C:3]1[CH:4]=[C:5]([S:9]([N:15]2[CH2:20][CH2:19][CH2:18][CH2:17][CH:16]2[CH2:21][OH:22])(=[O:11])=[O:10])[CH:6]=[CH:7][CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 94263Piperidin-2-ylmethanolHCID 27332503-(Trifluoromethyl)benzenesulfonyl chloride

생성물 1

HCID 5181860HCID 5181860, 화합물수율 28%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

3-(Trifluoromethyl)benzenesulfonic acid chloride (1 eq), dissolved in methylene chloride (65 ml), was added dropwise to a cooled solution (0° C.) of 2-piperidinemethanol (40 mmol, 1.1 eq) in methylene chloride (160 ml) and triethylamine (2.5 eq). When the addition was complete, the cooling bath was removed and the reaction mixture was stirred at room temperature until, according to thin layer chromatography control, the reaction was complete (90 min). Hydrogen chloride solution (0.5 mol/l, 75 ml) was added, the mixture was stirred for 15 min, the phases were separated and the organic phase was washed with water, dried over sodium sulfate and concentrated in vacuo. Yield: 28%

후처리

  1. additionWhen the addition
  2. customthe cooling bath was removed
  3. custom(90 min)
  4. additionHydrogen chloride solution (0.5 mol/l, 75 ml) was added
  5. stirringthe mixture was stirred for 15 min
  6. customthe phases were separated
  7. washthe organic phase was washed with water
  8. dry with materialdried over sodium sulfate
  9. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-b79cbd13708a4a4db28c4391c1e12819
출처 데이터셋
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08119805B2

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