Carbon Dioxide → Lithium 5-methyl-4,5,6,7-tetrahydrothiazolo[4,5-c]pyridine-2-carboxylate

HRID 352876ノート

反応式

HRID 352876 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][C:5]2[S:8][CH:9]=[N:10][C:4]=2[CH2:3]1.CCCCCC.C([Li:21])CCC.[C:22](=[O:24])=[O:23]>O1CCCC1>[CH3:1][N:2]1[CH2:7][CH2:6][C:5]2[S:8][C:9]([C:22]([O-:24])=[O:23])=[N:10][C:4]=2[CH2:3]1.[Li+:21]

参加物

6

反応物 4

HCID 280Carbon DioxideHCID 8058HexaneHCID 113786225-Methyl-4,5,6,7-tetrahydrothiazolo[4,5-c]pyridineHCID 178418339Butyllithium

生成物 1

HCID 23694153Lithium 5-methyl-4,5,6,7-tetrahydrothiazolo[4,5-c]pyridine-2-carboxylate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

In anhydrous tetrahydrofuran (10 ml) was dissolved 5-methyl-4,5,6,7-tetrahydrothiazolo[4,5-c]pyridine (583 mg), followed by the dropwise addition of a hexane solution (1.54M, 2.70 ml) of n-butyl lithium at −78° C. After stirring for 10 minutes, the reaction mixture was warmed up to 0° C. and stirring was conducted for 30 minutes. The reaction mixture was cooled to −78° C. A carbon dioxide gas was blown into the reaction mixture for 15 minutes, followed by warming up to room temperature. The reaction mixture was concentrated under reduced pressure, whereby the title compound (820 mg) was obtained as a pale brown foamy solid.

後処理

  1. stirringstirring
  2. waitwas conducted for 30 minutes
  3. temperatureThe reaction mixture was cooled to −78° C
  4. temperatureby warming up to room temperature
  5. concentrationThe reaction mixture was concentrated under reduced pressure, whereby the title compound (820 mg)
  6. customwas obtained as a pale brown foamy solid

出典と根拠

ORDレコード
ord-5832bbfc56ab4e57b883271f4e2550fd
出典データセット
uspto-grants-2004_06
特許番号
US06747023B1

反応ノート

読み込み中…