Ethanol → HCID 23033856、化合物

HRID 1393350ノート

反応式

HRID 1393350 の反応式
Br[C:2]1[S:3][C:4]2[C:10]([C:11]([OH:13])=[O:12])=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1.[NH:14]1[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1.C(O)C>C(OCC)C>[N:14]1([C:2]2[S:3][C:4]3[C:10]([C:11]([OH:13])=[O:12])=[CH:9][CH:8]=[CH:7][C:5]=3[N:6]=2)[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1

参加物

5

反応物 3

HCID 702EthanolHCID 8082PiperidineHCID 230338792-Bromo-1,3-benzothiazole-7-carboxylic acid

生成物 1

HCID 23033856HCID 23033856、化合物収率 90%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
72.5 °C

実験手順

A mixture of ethyl ester of 2-bromobenzothiazole-7-carboxylic acid (572 mg, 2.00 mmol), piperidine (5 ml) and ethanol (1 ml) was stirred at 70-75° C. for 2.5 hrs. Diethyl ether (15 ml) was added to the mixture at room temperature and the precipitates were filtered off and washed with diethyl ether. The filtrate and washings were combined and the solvent was distilled off under reduced pressure. The residue was purified by column chromatography on silica gel (chloroform) to give ethyl ester of 2-piperidinobenzothiazole-7-carboxylic acid (526 mg, 90%) as pale orange crystals.

後処理

  1. filtrationthe precipitates were filtered off
  2. washwashed with diethyl ether
  3. distillationthe solvent was distilled off under reduced pressure
  4. customThe residue was purified by column chromatography on silica gel (chloroform)

出典と根拠

ORDレコード
ord-81da932fa6cc48f284da6c53c1200355
出典データセット
uspto-grants-2008_03
特許番号
US07345068B2

反応ノート

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