1-(2-Aminoethyl)-4-(2-methoxyphenyl)piperazine → 3,4,5,6,7,8-Hexahydro-7-acetyl-3-[2-(4-(2-methoxyphenyl)-1-piperazinyl)ethyl]pyrido[4',3':4,5]thieno[2,3-d]pyrimidin-4-one

HRID 325080ノート

反応式

HRID 325080 の反応式
C(O[CH:4]=[N:5][C:6]1[S:17][C:9]2[CH2:10][N:11]([C:14](=[O:16])[CH3:15])[CH2:12][CH2:13][C:8]=2[C:7]=1[C:18]([O:20]CC)=O)C.[NH2:23][CH2:24][CH2:25][N:26]1[CH2:31][CH2:30][N:29]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][C:33]=2[O:38][CH3:39])[CH2:28][CH2:27]1>C(O)C>[C:14]([N:11]1[CH2:12][CH2:13][C:8]2[C:7]3[C:18](=[O:20])[N:23]([CH2:24][CH2:25][N:26]4[CH2:27][CH2:28][N:29]([C:32]5[CH:37]=[CH:36][CH:35]=[CH:34][C:33]=5[O:38][CH3:39])[CH2:30][CH2:31]4)[CH:4]=[N:5][C:6]=3[S:17][C:9]=2[CH2:10]1)(=[O:16])[CH3:15]

参加物

4

反応物 2

HCID 103991861-(2-Aminoethyl)-4-(2-methoxyphenyl)piperazineHCID 541290012-Ethoxymethyleneamino-3-carboethoxy-6-acetyl-4,5,6,7-tetrahydrothieno[2,3-c]pyridine

生成物 1

HCID 98046243,4,5,6,7,8-Hexahydro-7-acetyl-3-[2-(4-(2-methoxyphenyl)-1-piperazinyl)ethyl]pyrido[4',3':4,5]thieno[2,3-d]pyrimidin-4-one収率 80%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

5.8 g (23.4 mmol) of 2-ethoxymethyleneamino-3-carboethoxy-6-acetyl-4,5,6,7-tetrahydrothieno[2,3-c]pyridine in 50 ml of ethanol were mixed with 5.5 g (23.4 mmol) of 1-(2-aminoethyl)-4-(2-methoxyphenyl)piperazine and refluxed for 2 h. The mixture was then concentrated in a rotary evaporator, and the residue was taken up in 30 ml of ethyl acetate, heated to boiling and left to cool with stirring. The solid which crystallized out was filtered off with suction after cooling in an ice bath and was washed with ethyl acetate. 8.7 g (80%) of product with melting point 170-172° C. were isolated.

後処理

  1. temperaturerefluxed for 2 h
  2. concentrationThe mixture was then concentrated in a rotary evaporator
  3. temperatureheated
  4. waitleft
  5. temperatureto cool
  6. customThe solid which crystallized out
  7. filtrationwas filtered off with suction
  8. temperatureafter cooling in an ice bath
  9. washwas washed with ethyl acetate

出典と根拠

ORDレコード
ord-e06a8e4f27e14036a3f2cdafcfb2a921
出典データセット
uspto-grants-2001_04
特許番号
US06222034B1

反応ノート

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