Sodium borohydride → HCID 67338337, 화합물

HRID 82360

반응식

HRID 82360 반응식
[BH4-].[Na+].[Cl:3][C:4]1[CH:9]=[CH:8][C:7]([CH:10]=[C:11]([C:17]#[N:18])[C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:6][C:5]=1[F:19]>CCO>[Cl:3][C:4]1[CH:9]=[CH:8][C:7]([CH2:10][CH:11]([C:17]#[N:18])[C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:6][C:5]=1[F:19]

참가 물질

4

반응물 2

HCID 4311764Sodium borohydrideHCID 67338173Ethyl 3-(4-chloro-3-fluorophenyl)-2-cyanoacrylate

생성물 1

HCID 67338337HCID 67338337, 화합물수율 99%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

A solution NaBH4 (15 mg, 0.39 mmol) in EtOH (4 mL) was cannulated into a mixture of the ethyl 3-(4-chloro-3-fluorophenyl)-2-cyanoacrylate (200 mg, 0.79 mmol) in EtOH (2 mL) at room temperature. After 5 minutes, the mixture was quenched with 0.1N HCl, concentrated in vacuo, diluted with H2O, extracted with DCM, dried over MgSO4, concentrated and subject to flash chromatography (SiO2 with DCM) to give ethyl 3-(4-chloro-3-fluorophenyl)-2-cyanopropanoate (0.20 g, 58%). LCMS (APCI+) [M+H]+254.3.

후처리

  1. customthe mixture was quenched with 0.1N HCl
  2. concentrationconcentrated in vacuo
  3. additiondiluted with H2O
  4. extractionextracted with DCM
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-9a355cafe23f4371a3c41d7120267249
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846681B2

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