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

HRID 364420노트

반응식

HRID 364420 반응식
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

참가 물질

3

반응물 2

HCID 674Dimethylamine2회HCID 137264662-(2-Chloroethyl)-4-ethyl-2,3-dihydropyrido[3,2-f][1,4]oxazepin-5(4H)-thione hydrochloride

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-30a5161a9d6e454187d89cb47dfe394d
출처 데이터셋
uspto-grants-1986_08
특허 번호
US04604388

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