Hydrochloric Acid → 4-(4-Amino-6,7-dimethoxyquinazolin-2-yl)piperazine-1-imidic Acid Methyl Ester

HRID 461334노트

반응식

HRID 461334 반응식
[C:1]([N:3]1[CH2:8][CH2:7][N:6]([C:9]2[N:18]=[C:17]([NH2:19])[C:16]3[C:11](=[CH:12][C:13]([O:22][CH3:23])=[C:14]([O:20][CH3:21])[CH:15]=3)[N:10]=2)[CH2:5][CH2:4]1)#[N:2].[CH2:24]([O:26]CC)C.Cl.[OH-].[Na+]>CO>[CH3:24][O:26][C:1]([N:3]1[CH2:8][CH2:7][N:6]([C:9]2[N:18]=[C:17]([NH2:19])[C:16]3[C:11](=[CH:12][C:13]([O:22][CH3:23])=[C:14]([O:20][CH3:21])[CH:15]=3)[N:10]=2)[CH2:5][CH2:4]1)=[NH:2]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 14798Sodium HydroxideHCID 213933662-(4-Cyanopiperazin-1-yl)-4-amino-6,7-dimethoxyquinazoline

생성물 1

HCID 540910594-(4-Amino-6,7-dimethoxyquinazolin-2-yl)piperazine-1-imidic Acid Methyl Ester

시약·촉매·용매 1

HCID 887Methanol용매

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온도
0 °C

실험 절차

Under anhydrous conditions, 6.3 g. (0.02 mole) of 2-(4-cyanopiperazin-1-yl)-4-amino-6,7-dimethoxyquinazoline is dissolved in 150 ml. of ethyl ether and 1.8 ml. (0.044 mole) of reagent grade methanol is added. The solution is cooled to 0° C. and anhydrous hydrogen chloride is added until the solution is acid to Congo red paper. The resulting mixture is stored at 0° C. for 2 hours, then allowed to warm to room temperature (25° C) overnight. The reaction mixture is made alkaline with 2N sodium hydroxide, the ether layer separated, washed with 2 × 50 ml. of water, dried over anhydrous magnesium sulfate and evaporated to dryness to obtain the title compound.

후처리

  1. temperatureto warm to room temperature (25° C) overnight
  2. customthe ether layer separated
  3. washwashed with 2 × 50 ml
  4. dry with materialof water, dried over anhydrous magnesium sulfate
  5. customevaporated to dryness

출처 및 근거

ORD 기록
ord-bfb94a40fcda490093ddddb33ba7879b
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04062844

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