Succinic Acid → N-trityl piperazine, succinate salt

HRID 41863

反応式

HRID 41863 の反応式
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[C:7](Cl)([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[C:27]([OH:34])(=[O:33])[CH2:28][CH2:29][C:30]([OH:32])=[O:31]>C1(C)C=CC=CC=1.CO.C1(C)C=CC=CC=1>[C:27]([OH:34])(=[O:33])[CH2:28][CH2:29][C:30]([OH:32])=[O:31].[C:7]([N:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)([C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1)[C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1

参加物

6

反応物 3

HCID 1110Succinic AcidHCID 4837PiperazineHCID 6456Trityl chloride

生成物 1

HCID 67005131N-trityl piperazine, succinate salt収率 70%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 21867641Toluene methanol溶媒

実験手順

To a cooled solution of piperazine (10 eq) in toluene/methanol (5:1 toluene/methanol (v:v); 5 mL/g piperazine) was added slowly a solution of trityl chloride 10 (1.0 eq) in toluene (5 mL/g trityl chloride). Upon reaction completion (1-2 hr), this solution was washed four times with water. To the resulting organic solution was added an aqueous solution of succinic acid (1.1 eq; 13 mL water/g succinic acid). This mixture was stirred for 90 min, and the solid product was collected by filtration. The crude solid was purified by two reslurries in acetone. Yield=70%.

後処理

  1. customUpon reaction completion (1-2 hr)
  2. washthis solution was washed four times with water
  3. filtrationthe solid product was collected by filtration
  4. customThe crude solid was purified by two reslurries in acetone

出典と根拠

ORDレコード
ord-88f9cb7427b947d982fa3667e71af104
出典データセット
uspto-grants-2013_09
特許番号
US08536147B2

関連ノート

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