Water → HCID 68725377、化合物

HRID 1896011ノート

反応式

HRID 1896011 の反応式
[OH:1][C:2]1([CH2:15][C:16]#[C:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH2:7][CH2:6][N:5](C(OC(C)(C)C)=O)[CH2:4][CH2:3]1.FC(F)(F)C(O)=O.O.[OH-].[Na+]>C(Cl)(Cl)Cl>[C:18]1([C:17]#[C:16][CH2:15][C:2]2([OH:1])[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]2)[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1

参加物

6

反応物 4

HCID 962WaterHCID 6422Trifluoroacetic acidHCID 14798Sodium HydroxideHCID 86627346tert-Butyl 4-hydroxy-4-(3-phenylprop-2-ynyl)piperidine-1-carboxylate

生成物 1

HCID 68725377HCID 68725377、化合物収率 99.4%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
25 °C

実験手順

To a solution of Compound 256b (179 mg, 0.57 mmol) in CHCl3 (3 mL) was added trifluoroacetic acid (0.219 mL, 2.84 mmol) and the reaction mixture was then stirred at 25° C. for 24 h until the complete conversion of the reagent was observed by LC-MS. Afterwards, to the reaction mixture was added water, followed by aq. 2 N NaOH to give alkaline pH. Separation of the organic layer and extraction of the aqueous layer with CH2Cl2, washing the combined organic layers with brine and drying over Na2SO4 afforded the title compound (122 mg).

後処理

  1. customto give alkaline pH
  2. customSeparation of the organic layer and extraction of the aqueous layer with CH2Cl2
  3. washwashing the combined organic layers with brine
  4. dry with materialdrying over Na2SO4

出典と根拠

ORDレコード
ord-5e9a3e7e03b4414591dc7b6eb55d4543
出典データセット
uspto-grants-2013_08
特許番号
US08518916B2

反応ノート

読み込み中…