Chloroacetyl chloride → HCID 66958505, 화합물

HRID 1364028노트

반응식

HRID 1364028 반응식
[NH2:1][C:2]1[CH:3]=[N:4][C:5]2[C:10]([C:11]=1[NH:12][CH2:13][CH2:14][NH:15][C:16](=[O:22])[O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[CH:9][CH:8]=[CH:7][CH:6]=2.C(N(CC)CC)C.[Cl:30][CH2:31][C:32](Cl)=O>ClCCl>[Cl:30][CH2:31][C:32]1[N:12]([CH2:13][CH2:14][NH:15][C:16](=[O:22])[O:17][C:18]([CH3:19])([CH3:21])[CH3:20])[C:11]2[C:10]3[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=3[N:4]=[CH:3][C:2]=2[N:1]=1

참가 물질

5

반응물 3

HCID 6577Chloroacetyl chlorideHCID 8471TriethylamineHCID 12016824tert-Butyl 2-(3-aminoquinolin-4-ylamino)ethylcarbamate

생성물 1

HCID 66958505HCID 66958505, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A modification of the method described in Part E of Example 1 was used to treat tert-butyl 2-[(3-aminoquinolin-4-yl)amino]ethylcarbamate (15.65 g, 51.76 mmol) with triethylamine (10.82 mL, 77.64 mmol) followed by chloroacetyl chloride (4.5 mL, 57 mmol). The reaction was carried out in dichloromethane (60 mL). After the reaction mixture was filtered, the filtrate was washed with dilute aqueous sodium bicarbonate, dried over magnesium sulfate, and concentrated under reduced pressure to provide tert-butyl 2-[2-(chloromethyl)-1H-imidazo[4,5-c]quinolin-1-yl]ethylcarbamate as an amber-colored solid, which was combined with material from two other runs for use in the next step.

후처리

  1. filtrationAfter the reaction mixture was filtered
  2. washthe filtrate was washed with dilute aqueous sodium bicarbonate
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-7c1d5d6fd82f480e95afe213dc8c7192
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07888349B2

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