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Hydrochloric Acid → HCID 23371312, 화합물

HRID 1735704
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HRID 1735704 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[S:9][CH:10]=[C:11]([CH2:13][O:14][CH2:15][C:16]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[O:17])[N:12]=2)=[CH:4][CH:3]=1.[C:24](=O)([O:27]C)[O:25][CH3:26].[H-].[Na+].Cl>O1CCCC1.O.CO>[CH3:26][O:25][C:24]([CH:15]([O:14][CH2:13][C:11]1[N:12]=[C:8]([C:5]2[CH:4]=[CH:3][C:2]([F:1])=[CH:7][CH:6]=2)[S:9][CH:10]=1)[C:16]([C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1)=[O:17])=[O:27]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 12021Dimethyl CarbonateHCID 24758Sodium hydrideHCID 23371333HCID 23371333, 화합물

생성물 1

HCID 23371312HCID 23371312, 화합물수율 93.4%

시약·촉매·용매 3

HCID 887Methanol용매
HCID 962
Water
용매
HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 9.8 g (0.03 mol) of 2-[2-(4-fluorophenyl)-4-thiazolylmethyloxy]acetophenone in 80 ml of tetrahydrofuran is added dropwise to 3.0 g (0.033 mol) of dimethyl carbonate and 0.8 g (0.033 mol) of sodium hydride in 20 ml of tetrahydrofuran at 60° C. with stirring under nitrogen, and the mixture is then stirred at 60° C. for 1 hour. After cooling, first 5 ml of methanol and then 500 ml of water are added, and the mixture is acidified with dilute hydrochloric acid and extracted with methyl tert-butyl ether. The organic phase is washed with sodium bicarbonate solution, dried and concentrated. The result is 10.8 g (93% yield) of ω-methoxycarbonyl-2-[2-(4-fluorophenyl)-4-thiazolylmethyloxy]acetophenone as an ocher solid of melting point 86°-89° C.

후처리

  1. stirringthe mixture is then stirred at 60° C. for 1 hour
  2. temperatureAfter cooling
  3. extractionextracted with methyl tert-butyl ether
  4. washThe organic phase is washed with sodium bicarbonate solution
  5. customdried
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-1755a54ddebf468ea41b5d169e214234
출처 데이터셋
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05538940

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