Water → 3-(4-Methylpiperazin-1-yl)propyl (3-hydroxymethylphenyl)carbamate

HRID 1970859노트

반응식

HRID 1970859 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.[OH:8][CH2:9][C:10]1[CH:11]=[C:12]([NH:16][C:17](=[O:23])[O:18][CH2:19][CH2:20][CH2:21]Cl)[CH:13]=[CH:14][CH:15]=1.O.C(OCC)(=O)C>C(#N)C>[OH:8][CH2:9][C:10]1[CH:11]=[C:12]([NH:16][C:17](=[O:23])[O:18][CH2:19][CH2:20][CH2:21][N:5]2[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]2)[CH:13]=[CH:14][CH:15]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 531671-MethylpiperazineHCID 595647253-Chloropropyl (3-hydroxymethylphenyl)carbamate

생성물 1

HCID 595647273-(4-Methylpiperazin-1-yl)propyl (3-hydroxymethylphenyl)carbamate

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
65 °C

실험 절차

10 g (100 mmol) of N-methylpiperazine are added to a solution of 2.4 g (10 mmol) of 3-chloropropyl (3-hydroxymethylphenyl)carbamate in 10 ml of acetonitrile. The solution is refluxed for 4 h. The mixture is then hydrolysed by addition of water and cooled to about 65° C., and ethyl acetate is added. The mixture is then cooled to room temperature, during which the product is obtained as a solid between the organic and aqueous phases. The product is filtered off and rinsed with water, acetonitrile and ethyl acetate. The product is subsequently dried at 50° C. for several hours; ESI: 308 (M+H).

후처리

  1. temperatureThe solution is refluxed for 4 h
  2. temperatureThe mixture is then cooled to room temperature, during which the product
  3. customis obtained as a solid between the organic and aqueous phases
  4. filtrationThe product is filtered off
  5. washrinsed with water, acetonitrile and ethyl acetate
  6. customThe product is subsequently dried at 50° C. for several hours

출처 및 근거

ORD 기록
ord-ed3e98c6235c491e92708a170981fb1e
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08431572B2

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