Boron Trichloride → HCID 69211615, 화합물

HRID 30062노트

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HRID 30062 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 69211615HCID 69211615, 화합물수율 58.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-191cd4dbd06c46a684baff88706f32a3
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07423030B2

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