Potassium Carbonate → 1-[(Naphthalen-2-yl)methyl]-4-(1,3-thiazol-2-yl)piperazine

HRID 1763452

반응식

HRID 1763452 반응식
Br[CH2:2][C:3]1[CH:12]=[CH:11][C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=1.C(=O)([O-])[O-].[K+].[K+].[S:19]1[CH:23]=[CH:22][N:21]=[C:20]1[N:24]1[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]1>CN(C)C=O>[CH:4]1[C:5]2[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=2)[CH:11]=[CH:12][C:3]=1[CH2:2][N:27]1[CH2:28][CH2:29][N:24]([C:20]2[S:19][CH:23]=[CH:22][N:21]=2)[CH2:25][CH2:26]1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 703202-BromomethylnaphthaleneHCID 9118061-(Thiazol-2-yl)piperazine

생성물 1

HCID 203103421-[(Naphthalen-2-yl)methyl]-4-(1,3-thiazol-2-yl)piperazine수율 64.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
150 °C

실험 절차

To a solution of 22.1 g (0.1 mole) of 2-bromomethylnaphthalene in 150 ml of dimethylformamide, there were added successively 10.7 g (0.101 mole) of dry potassium carbonate and 17.2 g (0.101 mole) of 1-(2-thiazolyl)-piperazine. The resulting suspension was heated at 150° C. for 10 hours; the salt which had formed was then filtered off and the dimethylformamide was evaporated off under reduced pressure. There was obtained a brown crystalline residue which was washed with water and suction filtered off. The resulting 29 g of crystals were recrystallized in 150 ml of ethanol to give 20 g of 1-(2-naphthylmethyl)-4-(2-thiazolyl)-piperazine as beige crystals melting at 83°-84° C.

후처리

  1. customthe salt which had formed
  2. filtrationwas then filtered off
  3. customthe dimethylformamide was evaporated off under reduced pressure
  4. customThere was obtained a brown crystalline residue which
  5. washwas washed with water and suction
  6. filtrationfiltered off
  7. customThe resulting 29 g of crystals were recrystallized in 150 ml of ethanol

출처 및 근거

ORD 기록
ord-0952dee630b848dca5b8564c50eba470
출처 데이터셋
uspto-grants-1978_09
특허 번호
US04112092

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