Dimethylamine → 2-[2-(Dimethylamino)ethyl]-4-ethyl-2,3-dihydropyrido[3,2-f][1,4]oxazepin-5(4H)-thione

HRID 1194235ノート

反応式

HRID 1194235 の反応式
Cl.Cl[CH2:3][CH2:4][CH:5]1[CH2:11][N:10]([CH2:12][CH3:13])[C:9](=[S:14])[C:8]2[CH:15]=[CH:16][CH:17]=[N:18][C:7]=2[O:6]1.[CH3:19][NH:20][CH3:21]>>[CH3:19][N:20]([CH3:21])[CH2:3][CH2:4][CH:5]1[CH2:11][N:10]([CH2:12][CH3:13])[C:9](=[S:14])[C:8]2[CH:15]=[CH:16][CH:17]=[N:18][C:7]=2[O:6]1

参加物

3

反応物 2

HCID 674Dimethylamine2 回HCID 137264662-(2-Chloroethyl)-4-ethyl-2,3-dihydropyrido[3,2-f][1,4]oxazepin-5(4H)-thione hydrochloride

生成物 1

HCID 137265852-[2-(Dimethylamino)ethyl]-4-ethyl-2,3-dihydropyrido[3,2-f][1,4]oxazepin-5(4H)-thione

実験手順

2-(2-Chloroethyl)-4-ethyl-2,3-dihydropyrido[3,2-f][1,4]oxazepin-5(4H)-thione hydrochloride, 5.00 g (0.016 mole) was added to 20 ml of anhydrous dimethylamine. The reaction flask was sealed tightly and stirred at room temperature for 6 days. The flask was opened after cooling to 0° C. and dimethylamine allowed to evaporate at room temperature. The residue was taken up in chloroform (100 ml) and washed with dilute aqueous sodium hydroxide (1×30 ml). The chloroform layer was dried over sodium sulfate, filtered and concentrated by rotary evaporation. The residual oil was dissolved in hot cyclohexane. Upon cooling, 1.76 g (39.4%) of light yellow crystals were collected, m.p. 73° C.

後処理

  1. customThe reaction flask was sealed tightly
  2. temperatureafter cooling to 0° C.
  3. customto evaporate at room temperature
  4. washwashed with dilute aqueous sodium hydroxide (1×30 ml)
  5. dry with materialThe chloroform layer was dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated by rotary evaporation
  8. dissolutionThe residual oil was dissolved in hot cyclohexane
  9. temperatureUpon cooling
  10. custom1.76 g (39.4%) of light yellow crystals were collected

出典と根拠

ORDレコード
ord-b7bbad04e9cf49818d4bef418fecfce0
出典データセット
uspto-grants-1989_03
特許番号
US04812565

反応ノート

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