Boron Trichloride → HCID 69211615、化合物

HRID 30062ノート

反応式

HRID 30062 の反応式
C([O:8][CH2:9][C:10]1[C:19]2[C:14](=[CH:15][C:16]([O:20][CH3:21])=[CH:17][CH:18]=2)[C:13]([NH:22][CH:23]2[CH2:28][CH2:27][N:26]([CH2:29][C:30]3[CH:39]=[CH:38][C:37]4[C:32](=[CH:33][CH:34]=[CH:35][CH:36]=4)[CH:31]=3)[CH2:25][CH2:24]2)=[N:12][N:11]=1)C1C=CC=CC=1.B(Cl)(Cl)Cl.C(=O)(O)[O-].[Na+]>ClCCl>[OH:8][CH2:9][C:10]1[C:19]2[C:14](=[CH:15][C:16]([O:20][CH3:21])=[CH:17][CH:18]=2)[C:13]([NH:22][CH:23]2[CH2:28][CH2:27][N:26]([CH2:29][C:30]3[CH:39]=[CH:38][C:37]4[C:32](=[CH:33][CH:34]=[CH:35][CH:36]=4)[CH:31]=3)[CH2:25][CH2:24]2)=[N:12][N:11]=1

参加物

5

反応物 3

HCID 25135Boron TrichlorideHCID 516892Sodium BicarbonateHCID 692126684-benzyloxymethyl-7-methoxy-N-[1-(naphthalen-2-ylmethyl)piperidin-4-yl]phthalazin-1-amine

生成物 1

HCID 69211615HCID 69211615、化合物収率 58.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

A solution of 120 mg of 4-benzyloxymethyl-7-methoxy-N-[1-(naphthalen-2-ylmethyl)piperidin-4-yl]phthalazin-1-amine in 4 mL of dichloromethane is stirred under nitrogen at 0° C., followed by dropwise addition of 2.3 mL of a molar solution of boron trichloride in dichloromethane. The reaction medium is stirred for 1 hour at 0° C. and then for 30 minutes at room temperature. It is hydrolysed with aqueous sodium bicarbonate solution and extracted with dichloromethane. The organic phase is washed with water, dried over anhydrous sodium sulfate, filtered and evaporated under reduced pressure. The residue is purified on a column of silica (eluent: 100/0 to 85/15 v/v dichloromethane/methanol). 58 mg of product are obtained in the form of a beige-coloured powder.

後処理

  1. waitfor 30 minutes at room temperature
  2. extractionextracted with dichloromethane
  3. washThe organic phase is washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. customevaporated under reduced pressure
  7. customThe residue is purified on a column of silica (eluent: 100/0 to 85/15 v/v dichloromethane/methanol)

出典と根拠

ORDレコード
ord-191cd4dbd06c46a684baff88706f32a3
出典データセット
uspto-grants-2008_09
特許番号
US07423030B2

反応ノート

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