Ethanol → 1-acetyl-N-(2-benzothiazolyl)-4-piperidinemethanamine

HRID 579785

반응식

HRID 579785 반응식
[C:1]([N:4]1[CH2:9][CH2:8][CH:7]([CH2:10][NH:11][C:12]([NH:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[S:13])[CH2:6][CH2:5]1)(=[O:3])[CH3:2].ClC(Cl)(Cl)Cl.BrBr.C(O)C>C(#N)C>[C:1]([N:4]1[CH2:9][CH2:8][CH:7]([CH2:10][NH:11][C:12]2[S:13][C:20]3[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=3[N:14]=2)[CH2:6][CH2:5]1)(=[O:3])[CH3:2]

참가 물질

6

반응물 4

HCID 702EthanolHCID 5943Carbon TetrachlorideHCID 24408BromineHCID 14048941N-[(1-acetyl-4-piperidinyl)methyl]-N'-phenylthiourea

생성물 1

HCID 140489441-acetyl-N-(2-benzothiazolyl)-4-piperidinemethanamine

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a stirred mixture of 5.8 parts of N-[(1-acetyl-4-piperidinyl)methyl]-N'-phenylthiourea and 160 parts of tetrachloromethane were added 3.7 parts of bromine. The whole was stirred and refluxed for 15 minutes. After the additions of 16 parts of ethanol and 16 parts of acetonitrile, the reaction mixture was cooled. The precipitated product was filtered off, washed with acetonitrile and dried. The hydrobromide salt was dissolved in methanol and water. This solution was alkalized with ammonium hydroxide. The precipitated product was filtered off, washed with water and dried, yielding 2.7 parts of 1-acetyl-N-(2-benzothiazolyl)-4-piperidinemethanamine; mp. 138.1° C. (intermediate 29).

후처리

  1. temperaturerefluxed for 15 minutes
  2. filtrationThe precipitated product was filtered off
  3. washwashed with acetonitrile
  4. customdried
  5. dissolutionThe hydrobromide salt was dissolved in methanol
  6. filtrationThe precipitated product was filtered off
  7. washwashed with water
  8. customdried

출처 및 근거

ORD 기록
ord-23b81791d5794551ad8661db43ec02a3
출처 데이터셋
uspto-grants-1988_06
특허 번호
US04749702

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