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Triethylamine → HCID 21077851, 화합물

HRID 418453
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인쇄 미리보기

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HRID 418453 반응식
[Cl:1][C:2]1[CH:8]=[C:7]([F:9])[C:6]([CH3:10])=[CH:5][C:3]=1[NH2:4].[CH2:11](OCl)[CH2:12][CH2:13]C.CC[C:19](=[S:21])C.C(N(CC)CC)C>C(Cl)Cl>[Cl:1][C:2]1[CH:8]=[C:7]([F:9])[C:6]([CH3:10])=[C:5]2[C:3]=1[NH:4][C:12]([CH3:13])=[C:11]2[S:21][CH3:19]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 27248182-Chloro-4-fluoro-5-methylanilineHCID 95486922-ButanethioneHCID 13752033Butyl hypochlorite

생성물 1

HCID 21077851HCID 21077851, 화합물수율 67.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

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온도
-65 °C

실험 절차

A stirred solution of 2-chloro-4-fluoro-5-methylaniline (1.655 g) in methylene chloride (100 ml) under nitrogen was treated at −65° C. with a solution of butylhypochlorite (1.126 g) in methylene chloride (5 ml), stirred at −65° C. for 10 min, treated at −65° C. with a solution of methylthioacetone (1.080 g) in methylene chloride (5 ml) stirred at −65° C. for 1 hour, treated at −65° C. with triethylamine (1.05 g) and allowed to reach ambient temperature. The solution was washed, dried (MgSO4) and evaporated. The residue was purified by silica chromatography using 25% acetone in isohexane as eluent to give the sub-title compound (1.704 g).

후처리

  1. stirringstirred at −65° C. for 1 hour
  2. customto reach ambient temperature
  3. washThe solution was washed
  4. dry with materialdried (MgSO4)
  5. customevaporated
  6. customThe residue was purified by silica chromatography

출처 및 근거

ORD 기록
ord-30e3c6e8f87f47fdbced45e59d9b04e7
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08093278B2

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