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

HRID 1789491

反応式

HRID 1789491 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-ee56261ae4364f3eb952ade8c36ca8dd
出典データセット
uspto-grants-1987_08
特許番号
US04689330

関連ノート

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