Ethylenediamine → HCID 57732439, 화합물

HRID 1365069노트

반응식

HRID 1365069 반응식
F[C:2]1[CH:9]=[CH:8][C:7]([Br:10])=[CH:6][C:3]=1[CH:4]=O.[CH2:11]([NH2:14])[CH2:12][NH2:13]>O>[Br:10][C:7]1[CH:8]=[CH:9][C:2]2[NH:14][CH2:11][CH2:12][N:13]=[CH:4][C:3]=2[CH:6]=1

참가 물질

4

반응물 2

HCID 3301EthylenediamineHCID 7363275-Bromo-2-fluorobenzaldehyde

생성물 1

HCID 57732439HCID 57732439, 화합물

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
140 °C

실험 절차

A 5 mL microwave tube was charged with 2-fluoro-5-bromobenzaldehyde (1 g) and ethylenediamine (3 mL). The mixture was heated to 140° C. for 300 s using microwave irradiation. The reaction was diluted with water and extracted with diethyl ether. The organics were extracted with 1N HCl, and the pH of the aqueous layer was adjusted to ˜8 with 2.5M NaOH. The basic water layer was extracted again with diethyl ether. The organics were dried over magnesium sulfate, filtered and concentrated to dryness. Reconcentration from diethyl ether afforded 7-bromo-2,3-dihydro-1H-1,4-benzodiazepine as a yellow crystalline solid. H1 NMR (d6-dmso): 8.04 (s, 1H), 7.46 (d, 1H), 7.19 (dd, 1H), 7.07 (br t, 1H), 6.64 (d, 1H), 3.82 (m, 2H), 3.17 (m, 2H). Mass (ES+)=225.0 (100%).

후처리

  1. custommicrowave irradiation
  2. extractionextracted with diethyl ether
  3. extractionThe organics were extracted with 1N HCl
  4. extractionThe basic water layer was extracted again with diethyl ether
  5. dry with materialThe organics were dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated to dryness

출처 및 근거

ORD 기록
ord-ffe38f5e1ddf4e23b70707c1db4e9bdf
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07888503B2

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