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 1422616ノート

反応式

HRID 1422616 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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]−.

後処理

  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

出典と根拠

ORDレコード
ord-d6a96364eff5492a90bbc36ab79dee6c
出典データセット
uspto-grants-2015_01
特許番号
US08927531B2

反応ノート

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