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

HRID 352876노트

반응식

HRID 352876 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5832bbfc56ab4e57b883271f4e2550fd
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06747023B1

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