Bromine → HCID 67458099、化合物

HRID 1028108ノート

反応式

HRID 1028108 の反応式
[Br:1]Br.[S:3]1[CH:7]=[CH:6][N:5]=[C:4]1[N:8]1[CH2:13][CH2:12][CH:11]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH2:10][CH2:9]1>C(O)(=O)C.C(OCC)(=O)C>[Br:1][C:7]1[S:3][C:4]([N:8]2[CH2:13][CH2:12][CH:11]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH2:10][CH2:9]2)=[N:5][CH:6]=1

参加物

5

反応物 2

HCID 24408BromineHCID 60658779HCID 60658779、化合物

生成物 1

HCID 67458099HCID 67458099、化合物収率 97.4%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

Bromine (0.14 mL, 2.7 mmol) was weighed into a vial and then diluted with acetic acid (1 mL). This solution was added dropwise (over 10 minutes) to a solution of ethyl 1-(1,3-thiazol-2-yl)piperidine-4-carboxylate (650 mg, 2.7 mmol) in acetic acid (12.5 mL). The mixture was then diluted with ethyl acetate (100 mL) and washed with water (100 mL) and brine (100 mL). The organic layer was dried over sodium sulfate and concentrated in vacuo to provide 840 mg (2.63 mmol, 97% yield) of ethyl 1-(5-bromo-1,3-thiazol-2-yl)piperidine-4-carboxylate as a green oil.

後処理

  1. washwashed with water (100 mL) and brine (100 mL)
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-b430eadc81f14116948713a96529db0e
出典データセット
uspto-grants-2014_05
特許番号
US08735417B2

反応ノート

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