Potassium trimethylsilanolate → Potassium [(2S)-2-(3,5-difluorophenyl)-2,5,5-trimethyl-6-oxopiperidin-1-yl]acetate

HRID 1864924노트

반응식

HRID 1864924 반응식
[F:1][C:2]1[CH:3]=[C:4]([C@:9]2([CH3:23])[CH2:14][CH2:13][C:12]([CH3:16])([CH3:15])[C:11](=[O:17])[N:10]2[CH2:18][C:19]([O:21]C)=[O:20])[CH:5]=[C:6]([F:8])[CH:7]=1.C[Si](C)(C)[O-].[K+:29]>C1COCC1>[F:1][C:2]1[CH:3]=[C:4]([C@:9]2([CH3:23])[CH2:14][CH2:13][C:12]([CH3:15])([CH3:16])[C:11](=[O:17])[N:10]2[CH2:18][C:19]([O-:21])=[O:20])[CH:5]=[C:6]([F:8])[CH:7]=1.[K+:29]

참가 물질

4

반응물 2

HCID 23668039Potassium trimethylsilanolate2회HCID 57974130Methyl [(2S)-2-(3,5-difluorophenyl)-2,5,5-trimethyl-6-oxopiperidin-1-yl]acetate

생성물 1

HCID 66973013Potassium [(2S)-2-(3,5-difluorophenyl)-2,5,5-trimethyl-6-oxopiperidin-1-yl]acetate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of methyl [(2S)-2-(3,5-difluorophenyl)-2,5,5-trimethyl-6-oxopiperidin-1-yl]acetate from Step D (298 mg, 0.916 mmol) in THF (9 mL) at ambient temperature was added potassium trimethylsilanolate (147 mg, 1.14 mmol). The reaction was stirred for 24 hours and found to be incomplete by LCMS analysis. Additional quantities of potassium trimethylsilanolate were added as needed. The reaction was concentrated in vacuo to give a residue that required no further purification. MS: m/z=312 (M+1 for parent acid).

후처리

  1. concentrationThe reaction was concentrated in vacuo
  2. customto give a residue that
  3. customno further purification

출처 및 근거

ORD 기록
ord-6177c6ad38994a48844af600cfcb02a8
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07625901B2

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