4,5,6,7-Tetrahydro-2-methylthiazolo[5,4-c]pyridine → Potassium (2-methyl-4,5,6,7-tetrahydro-thiazolo[5,4-c]pyridin-5-yl)methyltrifluoroborate

HRID 1422616노트

반응식

HRID 1422616 반응식
[CH3:1][C:2]1[S:3][C:4]2[CH2:5][NH:6][CH2:7][CH2:8][C:9]=2[N:10]=1.Br[CH2:12][B-:13]([F:16])([F:15])[F:14].[K+:17]>O1CCCC1>[CH3:1][C:2]1[S:3][C:4]2[CH2:5][N:6]([CH2:12][B-:13]([F:16])([F:15])[F:14])[CH2:7][CH2:8][C:9]=2[N:10]=1.[K+:17]

참가 물질

4

반응물 2

HCID 150176454,5,6,7-Tetrahydro-2-methylthiazolo[5,4-c]pyridineHCID 23690312Potassium (bromomethyl)trifluoroborate

생성물 1

HCID 131732225Potassium (2-methyl-4,5,6,7-tetrahydro-thiazolo[5,4-c]pyridin-5-yl)methyltrifluoroborate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 2-methyl-4,5,6,7-tetrahydro-thiazolo[5,4-c]pyridine (3.00 g), potassium bromomethyltrifluoroborate (3.91 g), KHCO3 (1.95 g), KI (0.32 g), and tetrahydrofuran (25 mL) is stirred at reflux temperature for 4 h. After cooling to room temperature, the solvent is evaporated and the residue is suspended in acetone. The insoluble salts are separated by filtration and the filtrate is treated with diethyl ether. The precipitate is separated by filtration and dried to give the title compound (alternatively, the crude product is purified by chromatography on silica gel using dichloromethane and methanol as eluent). Mass spectrum (ESI−): m/z=235 [M]−.

후처리

  1. temperatureat reflux temperature for 4 h
  2. customthe solvent is evaporated
  3. customThe insoluble salts are separated by filtration
  4. additionthe filtrate is treated with diethyl ether
  5. customThe precipitate is separated by filtration
  6. customdried

출처 및 근거

ORD 기록
ord-d6a96364eff5492a90bbc36ab79dee6c
출처 데이터셋
uspto-grants-2015_01
특허 번호
US08927531B2

반응 노트

불러오는 중…