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Triethylamine → HCID 19010448, 화합물

HRID 1741592
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HRID 1741592 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:13]=[CH:14][CH:15]=1)[O:5][C:6]1[CH:7]=[N+:8]([O-])[CH:9]=[CH:10][CH:11]=1.C[Si]([C:20]#[N:21])(C)C.C(N(CC)CC)C>C(#N)C>[C:20]([C:7]1[C:6]([O:5][C:4]2[CH:13]=[CH:14][CH:15]=[C:2]([F:1])[CH:3]=2)=[CH:11][CH:10]=[CH:9][N:8]=1)#[N:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 82115Trimethylsilyl cyanideHCID 19010447HCID 19010447, 화합물

생성물 1

HCID 19010448HCID 19010448, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 33.44 g of 3-(3-fluorophenoxy)pyridine N-oxide, 64.6 ml of trimethylsilyl cyanide and 45.9 ml of triethylamine in 180 ml of acetonitrile was refluxed for 4 hours. After the reaction mixture was concentrated, 200 ml of methylene chloride and 100 ml of 2M aqueous potassium carbonate was added to the residue and the mixture was stirred for a few minutes. The organic layer separated was washed with 50 ml of water, dried over anhydrous sodium sulfate, and concentrated. The solid obtained was washed with isopropyl ether to yield 28.30 g of pale brown crystals, which were recrystallized from ethyl acetate to give slightly brown crystals, mp 92°-93° C.

후처리

  1. temperaturewas refluxed for 4 hours
  2. concentrationAfter the reaction mixture was concentrated
  3. addition200 ml of methylene chloride and 100 ml of 2M aqueous potassium carbonate was added to the residue
  4. customThe organic layer separated
  5. washwas washed with 50 ml of water
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated
  8. customThe solid obtained
  9. washwas washed with isopropyl ether

출처 및 근거

ORD 기록
ord-9c1aad21690c4276aef1732f1bb6809d
출처 데이터셋
uspto-grants-1994_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05334594

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