4-Toluenesulfonyl chloride → 4,7-Bis(p-tolylsulphonyl)-1,4,7-triazacyclononane

HRID 1935346ノート

反応式

HRID 1935346 の反応式
N1CCNCCNCC1.[C:10]1(C)[CH:15]=CC(S(Cl)(=O)=O)=C[CH:11]=1.[C:21]1([CH3:49])[CH:26]=[CH:25][C:24]([S:27]([N:30]2[CH2:38][CH2:37][NH:36][CH2:35][CH2:34][N:33]([S:39]([C:42]3[CH:47]=[CH:46][C:45]([CH3:48])=[CH:44][CH:43]=3)(=[O:41])=[O:40])[CH2:32][CH2:31]2)(=[O:29])=[O:28])=[CH:23][CH:22]=1.ICCCI.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[C:21]1([CH3:49])[CH:26]=[CH:25][C:24]([S:27]([N:30]2[CH2:38][CH2:37][NH:36][CH2:35][CH2:34][N:33]([S:39]([C:42]3[CH:47]=[CH:46][C:45]([CH3:48])=[CH:44][CH:43]=3)(=[O:40])=[O:41])[CH2:32][CH2:31]2)(=[O:29])=[O:28])=[CH:23][CH:22]=1.[CH3:11][CH2:10][CH3:15].[C:21]1([CH3:49])[CH:26]=[CH:25][C:24]([S:27]([N:30]2[CH2:38][CH2:37][NH:36][CH2:35][CH2:34][N:33]([S:39]([C:42]3[CH:47]=[CH:46][C:45]([CH3:48])=[CH:44][CH:43]=3)(=[O:40])=[O:41])[CH2:32][CH2:31]2)(=[O:29])=[O:28])=[CH:23][CH:22]=1

参加物

8

反応物 5

HCID 73974-Toluenesulfonyl chlorideHCID 11430Potassium CarbonateHCID 123141,3-DiiodopropaneHCID 1883181,4,7-TriazacyclononaneHCID 109062624,7-Bis(p-tolylsulphonyl)-1,4,7-triazacyclononane

生成物 2

HCID 109062624,7-Bis(p-tolylsulphonyl)-1,4,7-triazacyclononaneHCID 17939386HCID 17939386、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

N,N′-bis(p-toluenesulfonyl)-1,4,7-triazacyclononane (1.1.20) was prepared by reacting (1.1.3) with two equivalents of p-toluenesulfonyl chloride. Two equivalents of N,N′-bis(p-toluenesulfonyl)-1,4,7-triazacyclononane (1.1.20) hydrobromide were reacted with one equivalent of 1,3-diiodopropane in acetonitrile with excess potassium carbonate. 1,3-Bis[N,N′-bis(p-toluenesulfonyl)-1,4,7-triazacyclononane propane (1.1.21) was isolated and purified by chromatography. The p-toluenesulfonyl groups were removed using sulfuric acid and HBr to yield the title compound (1.1.19).

出典と根拠

ORDレコード
ord-b718a5cbb0b444359a2bff50bdcc59e6
出典データセット
uspto-grants-2002_05
特許番号
US06387891B2

反応ノート

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