Barium hydroxide → HCID 39733728, 화합물

HRID 1808335노트

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HRID 1808335 반응식
[OH-:1].[Ba+2].[OH-:3].O1CCN([C:10](=S)[CH2:11][C:12]2[CH:21]=[C:20]3[C:15]([CH2:16][CH2:17][CH2:18][NH:19]3)=[CH:14][CH:13]=2)CC1>C(O)C>[NH:19]1[C:20]2[C:15](=[CH:14][CH:13]=[C:12]([CH2:11][C:10]([OH:3])=[O:1])[CH:21]=2)[CH2:16][CH2:17][CH2:18]1

참가 물질

4

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온도
80 °C

실험 절차

110 ml of a 20% barium hydroxide solution were added dropwise to a solution of 1-morpholino-2-(1,2,3,4-tetrahydroquinolin-7-yl)-ethanethione (11 g; 1 equiv.) in 55 ml of ethanol, and the resulting reaction mixture was heated for 10 hours at reflux. When the conversion was complete, the solvent was removed under reduced pressure and the residue was taken up in 100 ml of water and heated to 80° C. The reaction mixture was then neutralised carefully with dry ice, filtered over Celite and concentrated under reduced pressure. The resulting crude product (14 g) was used in the next stage without further purification.

후처리

  1. customthe resulting reaction mixture
  2. temperaturewas heated for 10 hours
  3. temperatureat reflux
  4. customthe solvent was removed under reduced pressure
  5. filtrationfiltered over Celite
  6. concentrationconcentrated under reduced pressure
  7. customThe resulting crude product (14 g) was used in the next stage without further purification

출처 및 근거

ORD 기록
ord-b969773ccd7b4931822e4bb147008098
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08357717B2

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