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Ethanolamine → HCID 58046394, 화합물

HRID 2046388
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HRID 2046388 반응식
[CH2:1]([CH2:3][NH2:4])[OH:2].Cl[C:6]1[N:7]=[N:8][CH:9]=[C:10]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)[CH:11]=1.C(OCC)(=O)C.O>O1CCOCC1>[F:18][C:15]1[CH:14]=[CH:13][C:12]([C:10]2[CH:11]=[C:6]([NH:4][CH2:3][CH2:1][OH:2])[N:7]=[N:8][CH:9]=2)=[CH:17][CH:16]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 700Ethanolamine2회HCID 962WaterHCID 8857Ethyl AcetateHCID 58046417HCID 58046417, 화합물

생성물 1

HCID 58046394HCID 58046394, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
120 °C

실험 절차

Ethanolamine (4.82 mL, 80 mmol) was added to a stirred mixture of 3-chloro-5-(4-fluorophenyl)pyridazine (2.08 g, 9.97 mmol) in Dioxane (40 mL) in a sealed tube. The mixture was heated to 120° C. overnight, treated with additional ethanolamine (1.2 mL, 20 mmol), and heated to 150° C. for 2 h. The mixture was cooled and poured into ethyl acetate (100 mL) and water (100 mL). The precipitate was filtered and dried to afford the title compound. 1H NMR (500 MHz, CD3SOCD3) δ 8.76 (d, 1H); 7.78 (dd, 2H); 7.36 (t, 2H); 7.02 (d, 1H); 6.85 (t, 1H); 4.78 (t, 1H); 3.58 (q, 2H); 3.45 (q, 2H). LRMS (APCI) calc'd for (C12H13FN3O) [M+H]+, 234.1. found 234.1.

후처리

  1. temperatureheated to 150° C. for 2 h
  2. temperatureThe mixture was cooled
  3. filtrationThe precipitate was filtered
  4. customdried

출처 및 근거

ORD 기록
ord-3122348ec4b240bb87cc0ad1e3db917e
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08592425B2

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