Potassium Carbonate → HCID 68872701、化合物

HRID 2112036ノート

反応式

HRID 2112036 の反応式
Br[CH2:2][CH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])[CH:5]=1.[C:15]([O:24][CH3:25])(=[O:23])[C:16]1[C:17](=[CH:19][CH:20]=[CH:21][CH:22]=1)[SH:18].C([O-])([O-])=O.[K+].[K+]>C(#N)C>[C:11]([O:10][C:6]1[CH:5]=[C:4]([CH2:3][CH2:2][S:18][C:17]2[CH:19]=[CH:20][CH:21]=[CH:22][C:16]=2[C:15]([O:24][CH3:25])=[O:23])[CH:9]=[CH:8][CH:7]=1)([CH3:14])([CH3:13])[CH3:12]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 21009Benzoic acid, 2-mercapto-, methyl esterHCID 68872917HCID 68872917、化合物

生成物 1

HCID 68872701HCID 68872701、化合物収率 98.2%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

1-(2-Bromoethyl)-3-tert-butoxybenzene (320 mg, 1.244 mmol) was dissolved in acetonitrile (15 ml). Methyl thiosalicylate (209 mg, 1.244 mmol) was added and then potassium carbonate, anhydrous (258 mg, 1.866 mmol) was added. The mixture was heated to reflux for 3 hours and then evaporated under vacuum to dryness. Chromatography of the residue on a column (ISOLUTE® SI, 5 g/25 ml) using ethyl acetate/heptane (5:95) as eluant gave 421 mg desired product, yield 98%.

後処理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 3 hours
  3. customevaporated under vacuum to dryness

出典と根拠

ORDレコード
ord-f496b5a7aff04dac869fa2c8a8c1c207
出典データセット
uspto-grants-2009_04
特許番号
US07521461B2

反応ノート

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