Potassium Carbonate → HCID 21933594, 화합물

HRID 1370169노트

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HRID 1370169 반응식
C(=O)([O-])[O-].[K+].[K+].Br[CH2:8][CH2:9][C:10]([OH:12])=[O:11].[SH:13][C:14]1[CH:23]=[C:22]([Cl:24])[CH:21]=[CH:20][C:15]=1[C:16]([O:18][CH3:19])=[O:17]>CC(C)=O>[OH:12][C:10]([CH2:9][CH2:8][S:13][C:14]1[CH:23]=[C:22]([Cl:24])[CH:21]=[CH:20][C:15]=1[C:16]([O:18][CH3:19])=[O:17])=[O:11]

참가 물질

5

실험 절차

179.5 g (1.3 mol) of potassium carbonate and, a little at a time, 94.5 g (0.62 mol) of 3-bromopropionic acid were added to a solution of 125.4 g (0.62 mol) of methyl 2-mercapto-4-chlorobenzoate in 1.5 l of acetone, and the reaction mixture was stirred at room temperature for 12 hours. The solvent was distilled off, the residue was taken up in water and the mixture was extracted with diethyl ether. The aqueous phase was then made acidic using concentrated hydrochloric acid and the precipitate was filtered off with suction and dried. This gave 160 g (88%) of methyl 2-(2-hydroxycarbonyeth-1-yl)thio-4-chlorobenzoate M.p.: 133 to 136° C.

후처리

  1. distillationThe solvent was distilled off
  2. extractionthe mixture was extracted with diethyl ether
  3. filtrationthe precipitate was filtered off with suction
  4. customdried

출처 및 근거

ORD 기록
ord-6eaed12f90fb4c01b1ea2eaed373a234
출처 데이터셋
uspto-grants-2003_06
특허 번호
US06583089B1

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