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Potassium Carbonate → HCID 13117186, 화합물

HRID 851279
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HRID 851279 반응식
[Cl:1][C:2]1[CH:23]=[CH:22][C:5]2[N:6]=[C:7]([O:9][C:10]3[CH:21]=[CH:20][C:13]([O:14][CH:15]([CH3:19])[C:16]([OH:18])=[O:17])=[CH:12][CH:11]=3)[S:8][C:4]=2[CH:3]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH:31]1[CH2:36][CH2:35][O:34][C:32]1=[O:33]>CC(C)=O>[Cl:1][C:2]1[CH:23]=[CH:22][C:5]2[N:6]=[C:7]([O:9][C:10]3[CH:21]=[CH:20][C:13]([O:14][CH:15]([CH3:19])[C:16]([O:18][CH:31]4[CH2:36][CH2:35][O:34][C:32]4=[O:33])=[O:17])=[CH:12][CH:11]=3)[S:8][C:4]=2[CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 954632(3H)-Furanone, 3-bromodihydro-HCID 156003Fenthiaprop

생성물 1

HCID 13117186HCID 13117186, 화합물

시약·촉매·용매 1

HCID 180Acetone용매2회

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온도
45 °C

실험 절차

21 g (0.06 mole) of 2-[4-(6-chloro-2-benzthiazolyloxy)-phenoxy]-propionic acid were initially taken together with 10.4 g (0.075 mole) of potassium carbonate in 100 ml of acetone and the mixture was stirred for approx. 1/2 hour at 45° C., a thick paste being formed. 11.6 g (0.07 mole) of 2-bromobutyrolactone in 50 ml of acetone were then added dropwise in the course of 1/2 hour. When the addition was complete, the reaction mixture became highly fluid; the conversion was followed by means of thin-layer chromatography and was approx. 70% after 5 hours. Altogether, the mixture was stirred for 16 hours at approx. 50° C. After cooling, the salt was filtered off, the acetone was removed by distillation and the residue was taken up in approx. 200 ml of toluene and washed with water and saturated sodium bicarbonate solution. After drying, the toluene was removed by distillation and the residue remaining was dried in vacuo (0.05 mbar) for one hour at approx. 70° C. The product remaining after drying was 22 g (91.3% of theory) of a very viscous oil, which was identified by 1H nuclear magnetic resonance spectroscopy as 2-oxotetrahydrofuran-3-yl 2-[4-(6-benzthiazolyloxy)-phenoxy]-propanoate. ##STR12##

후처리

  1. customa thick paste being formed
  2. additionWhen the addition
  3. customafter 5 hours
  4. stirringAltogether, the mixture was stirred for 16 hours at approx. 50° C
  5. temperatureAfter cooling
  6. filtrationthe salt was filtered off
  7. customthe acetone was removed by distillation
  8. washwashed with water and saturated sodium bicarbonate solution
  9. customAfter drying
  10. customthe toluene was removed by distillation
  11. customthe residue remaining was dried in vacuo (0.05 mbar) for one hour at approx. 70° C
  12. customafter drying

출처 및 근거

ORD 기록
ord-f519f35a163846bc90df2d142f4a8d03
출처 데이터셋
uspto-grants-1983_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04383850

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