Ethylenediamine → HCID 57732439、化合物

HRID 1365069ノート

反応式

HRID 1365069 の反応式
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

参加物

4

反応物 2

HCID 3301EthylenediamineHCID 7363275-Bromo-2-fluorobenzaldehyde

生成物 1

HCID 57732439HCID 57732439、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
140 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-ffe38f5e1ddf4e23b70707c1db4e9bdf
出典データセット
uspto-grants-2011_02
特許番号
US07888503B2

反応ノート

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