Potassium Carbonate → HCID 21933594、化合物

HRID 1370169ノート

反応式

HRID 1370169 の反応式
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]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 115533-Bromopropionic acidHCID 1565712452948-12-6

生成物 1

HCID 21933594HCID 21933594、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-6eaed12f90fb4c01b1ea2eaed373a234
出典データセット
uspto-grants-2003_06
特許番号
US06583089B1

反応ノート

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