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Sodium Iodide → HCID 67407516, 화합물

HRID 2068844
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HRID 2068844 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([NH2:8])[CH:5]=[C:4]([C:9]([F:12])([F:11])[F:10])[C:3]=1[NH2:13].Cl[CH2:15][CH2:16][O:17][CH2:18][CH2:19]Cl.[I-].[Na+]>C(#N)C>[Cl:1][C:2]1[CH:7]=[C:6]([N:8]2[CH2:19][CH2:18][O:17][CH2:16][CH2:15]2)[CH:5]=[C:4]([C:9]([F:12])([F:11])[F:10])[C:3]=1[NH2:13]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 5238Sodium IodideHCID 8115Bis(2-chloroethyl) etherHCID 67406226HCID 67406226, 화합물

생성물 1

HCID 67407516HCID 67407516, 화합물수율 24%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
165 °C

실험 절차

2-Chloro-6-trifluoromethyl-benzene-1,4-diamine (2.9 g), bis-(2-chloroethyl)ether (1.7 mL) and sodium iodide (516 mg) were mixed in acetonitrile (45 mL) and heated to 165° C. for 1 hour in a sealed microwave process vessel. The crude mixture was concentrated in vacuo, redissolved in ethyl acetate (100 mL) and washed with water (2×100 mL) and brine (1×100 mL). The organic phase was dried over magnesium sulfate and concentrated in vacuo. The crude product was purified by flash chromatography to furnish 940 mg (24%) of the title compound as a black oil. 1H NMR (500 MHz, CDCl3): 3.02 (m, 4H), 3.84 (m, 4H), 4.30 (b, 2H), 6.97 (d, 1H), 7.06 (d, 1H).

후처리

  1. concentrationThe crude mixture was concentrated in vacuo
  2. dissolutionredissolved in ethyl acetate (100 mL)
  3. washwashed with water (2×100 mL) and brine (1×100 mL)
  4. dry with materialThe organic phase was dried over magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe crude product was purified by flash chromatography

출처 및 근거

ORD 기록
ord-26a77343bb584d1e93ee3774c5fddd12
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08299075B2

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