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Triethylamine → HCID 68128176, 화합물

HRID 1077045
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HRID 1077045 반응식
[CH2:1]1[C:11]2[N:10]3[C:12]4[CH:21]=[CH:20][N:19]=[CH:18][C:13]=4[C:14]4[CH2:15][CH2:16][CH:17]=[C:8]([C:9]=43)[CH:7]=[CH:6][C:5]=2[CH2:4][CH2:3][CH2:2]1.C(N(CC)CC)C.C(Cl)(=[O:33])C(C)C>ClCCl>[CH:8]([C:9]([CH:14]([CH3:15])[CH3:13])=[O:33])([CH3:17])[CH3:7].[CH2:1]1[C:11]2[N:10]3[C:12]4[CH:21]=[CH:20][N:19]=[CH:18][C:13]=4[C:14]4[CH2:15][CH2:16][CH:17]=[C:8]([C:9]=43)[CH:7]=[CH:6][C:5]=2[CH2:4][CH2:3][CH2:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 62325Isobutyryl chlorideHCID 67838308HCID 67838308, 화합물

생성물 1

HCID 68128176HCID 68128176, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 5.5 g. of the product of Example 1 in 150 ml. of dichloromethane containing 25 ml. of triethylamine a solution of 4.2 ml. of isobutyryl chloride in approximately 25 ml. of dichloromethane is added dropwise, with constant stirring. On heating to reflux, the white precipitate originally formed redissolves. Refluxing is continued for 2 hours; the solution is cooled, washed with water and with saturated sodium bicarbonate, dried over anhydrous potassium carbonate, and stripped down to a dark gum, which is taken up in hexane, boiled and decolorized. After concentrating the clear solution tp 100 ml. and cooling, a gum separates which solidifies completely on standing. After 1 week, 1,2,3,4,8,9-hexahydropyrido[4', 3':2,3]indolo[1,7-ab][1]benzazepin isopropyl ketone, m.p. 122°-124°, is isolated.

후처리

  1. temperatureOn heating
  2. temperatureto reflux
  3. customthe white precipitate originally formed
  4. dissolutionredissolves
  5. temperatureRefluxing
  6. temperaturethe solution is cooled
  7. washwashed with water and with saturated sodium bicarbonate
  8. dry with materialdried over anhydrous potassium carbonate
  9. concentrationAfter concentrating the clear solution tp 100 ml
  10. temperatureand cooling
  11. waitAfter 1 week

출처 및 근거

ORD 기록
ord-680c4511925145ba88b8d615c3dd5784
출처 데이터셋
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03959300

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