Potassium Carbonate → HCID 68872701, 화합물

HRID 2112036노트

반응식

HRID 2112036 반응식
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]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 21009Benzoic acid, 2-mercapto-, methyl esterHCID 68872917HCID 68872917, 화합물

생성물 1

HCID 68872701HCID 68872701, 화합물수율 98.2%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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%.

후처리

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

출처 및 근거

ORD 기록
ord-f496b5a7aff04dac869fa2c8a8c1c207
출처 데이터셋
uspto-grants-2009_04
특허 번호
US07521461B2

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