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

HRID 1367246ノート

反応式

HRID 1367246 の反応式
[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]

参加物

4

反応物 2

HCID 23668039Potassium trimethylsilanolate2 回HCID 57974130Methyl [(2S)-2-(3,5-difluorophenyl)-2,5,5-trimethyl-6-oxopiperidin-1-yl]acetate

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-f76b992b829e427b9ed26a58772f489b
出典データセット
uspto-grants-2011_02
特許番号
US07893079B2

反応ノート

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