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 325080노트

반응식

HRID 325080 반응식
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]

참가 물질

4

반응물 2

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

생성물 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-one수율 80%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e06a8e4f27e14036a3f2cdafcfb2a921
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06222034B1

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