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Methyl iodide → 2-(1-Methoxyethyl)-1,4-bis(phenylmethyl)piperazine

HRID 35315
ノート
印刷プレビュー

反応式

HRID 35315 の反応式
[CH3:1][CH:2]([CH:4]1[CH2:9][N:8]([CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH2:7][CH2:6][N:5]1[CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[OH:3].[H-].[Na+].I[CH3:27]>CN(C)C=O>[CH3:27][O:3][CH:2]([CH:4]1[CH2:9][N:8]([CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH2:7][CH2:6][N:5]1[CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[CH3:1]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 21295699(1,4-Dibenzyl-piperazin-2-yl)-ethanol

生成物 1

HCID 212957062-(1-Methoxyethyl)-1,4-bis(phenylmethyl)piperazine収率 71.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a stirred mixture of 60.5 parts of α-methyl-1,4-bis(phenylmethyl)-2-piperazinemethanol and 180 parts of N,N-dimethylformamide were added portionwise 29.8 parts of a sodium hydride dispersion 50% at a temperature below 35° C. under nitrogen atmosphere. The mixture was allowed to cool and stirred for 3 hours at room temperature. After cooling to 10° C., there were added dropwise 9.4 parts of iodomethane at about 20° C. Upon completion, stirring was continued for 2 hours at room temperature. The reaction mixture was poured onto water and the product was extracted twice with 1,1'-oxybisethane. The combined extracts were washed with water, dried, filtered and evaporated, yielding 45.2 parts (71.5%) of 2-(1-methoxyethyl)-1,4-bis(phenylmethyl)piperazine as a residue (intermediate 28).

後処理

  1. temperatureto cool
  2. temperatureAfter cooling to 10° C.
  3. stirringUpon completion, stirring
  4. waitwas continued for 2 hours at room temperature
  5. additionThe reaction mixture was poured onto water
  6. extractionthe product was extracted twice with 1,1'-oxybisethane
  7. washThe combined extracts were washed with water
  8. customdried
  9. filtrationfiltered
  10. customevaporated

出典と根拠

ORDレコード
ord-de2efa54aeb44026a641832766aa2f0a
出典データセット
uspto-grants-1988_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04766125

反応ノート

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