Triethylamine → HCID 86748235, 화합물

HRID 2379394노트

반응식

HRID 2379394 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]=[N:10][C:11](Br)=[CH:12][C:13]=2[OH:14])=[CH:4][CH:3]=1.C(N(CC)CC)C.[C:23]([Cl:30])(=[O:29])[S:24][CH2:25][CH2:26][CH2:27][CH3:28]>C1C=CC=CC=1>[C:23](=[O:29])([O-:14])[S:24][CH2:25][CH2:26][CH2:27][CH3:28].[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]=[N:10][C:11]([Cl:30])=[CH:12][C:13]=2[OH:14])=[CH:4][CH:3]=1

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 13295035S-Butyl carbonochloridothioateHCID 178515449HCID 178515449, 화합물

생성물 2

HCID 86748235HCID 86748235, 화합물HCID 178516196HCID 178516196, 화합물

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

3-(4'-Chlorophenyl)-4-hydroxy-6-bromopyridazine (14.2 g, 0.0497 mol) was suspended in 100 ml of benzene, triethylamine (5.5 g, 0.0543 mol) was added, and the mixture was stirred for 3.5 hours at room temperature to complete the reaction. S-Butyl thiochlorocarbonate (7.85 g, 0.05162 mol) was then added dropwise to the mixture in the course of 5 minutes, and the reaction mixture was stirred for 3 more hours without heating. The triethylamine hydrochloride which had precipitated was filtered off, and the benzene solution was washed in succession in each case with 150 ml portions of water, highly dilute hydrochloric acid, highly dilute sodium hydroxide solution and then again water, and dried over sodium sulfate. The solvent was then removed completely in vacuo, and finally under an oil-pump vacuum (0.2 Torr, 90° C. bath temperature). The S-butyl thiocarbonate of 3-(4'-chlorophenyl)-4-hydroxy-6-chloropyridazine, which was first obtained as an oil (17.5 g, 0.04356 mol, 87.6% of theory), solidified upon prolonged standing and, when dissolved in and allowed to crystallize from hexane, showed amp. of 68°-71° C.

후처리

  1. customthe reaction
  2. stirringthe reaction mixture was stirred for 3 more hours
  3. temperaturewithout heating
  4. customThe triethylamine hydrochloride which had precipitated
  5. filtrationwas filtered off
  6. washthe benzene solution was washed in succession in each case with 150 ml portions of water, highly dilute hydrochloric acid, highly dilute sodium hydroxide solution
  7. dry with materialagain water, and dried over sodium sulfate
  8. customThe solvent was then removed completely in vacuo
  9. customfinally under an oil-pump vacuum (0.2 Torr, 90° C. bath temperature)

출처 및 근거

ORD 기록
ord-3266497d9faf4e908792c2687ff2706e
출처 데이터셋
uspto-grants-1994_11
특허 번호
US05362708

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