Potassium Carbonate → HCID 178491756、化合物

HRID 1517386ノート

反応式

HRID 1517386 の反応式
Cl[CH2:2][C:3]1[C:8]2[NH:9][C:10]([CH2:12][N:13]([CH3:27])[S:14]([C:17]3[C:22]([CH3:23])=[CH:21][C:20]([O:24][CH3:25])=[CH:19][C:18]=3[CH3:26])(=[O:16])=[O:15])=[N:11][C:7]=2[CH:6]=[CH:5][CH:4]=1.C([O-])([O-])=O.[K+].[K+].Cl.Cl.[N:36]1[CH:41]=[CH:40][C:39]([N:42]2[CH2:52][CH2:51][C:45]3([CH2:50][CH2:49][NH:48][CH2:47][CH2:46]3)[CH2:44][CH2:43]2)=[CH:38][CH:37]=1>CC(C)=O>[CH3:25][O:24][C:20]1[CH:21]=[C:22]([CH3:23])[C:17]([S:14]([N:13]([CH3:27])[CH2:12][C:10]2[NH:9][C:8]3[C:3]([CH2:2][N:48]4[CH2:47][CH2:46][C:45]5([CH2:51][CH2:52][N:42]([C:39]6[CH:40]=[CH:41][N:36]=[CH:37][CH:38]=6)[CH2:43][CH2:44]5)[CH2:50][CH2:49]4)=[CH:4][CH:5]=[CH:6][C:7]=3[N:11]=2)(=[O:16])=[O:15])=[C:18]([CH3:26])[CH:19]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 66701057HCID 66701057、化合物HCID 178491755HCID 178491755、化合物

生成物 1

HCID 178491756HCID 178491756、化合物収率 25%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of N-((7-(chloromethyl)-1H-benzo[d]imidazol-2-yl)methyl)-4-methoxy-N,2,6-trimethylbenzenesulfonamide (0.74 mmol, 1.0 eq.), K2CO3 (2.5 eq.) and 9-pyridin-4-Yl-3,9-diazaspiro[5.5]undecane dihydrochloride (AMN-01) (0.88 mmol, 1.2 eq.) in abs. acetone (20 ml) was heated under reflux for 16 h. The reaction mixture was filtered off and the filtrate was concentrated in order to obtain the crude product, which was purified by column chromatography over neutral aluminium oxide. Yield: 25%

後処理

  1. temperatureunder reflux for 16 h
  2. filtrationThe reaction mixture was filtered off
  3. concentrationthe filtrate was concentrated in order

出典と根拠

ORDレコード
ord-42392fb438ee4f46b74ff7662e8b6d32
出典データセット
uspto-grants-2012_07
特許番号
US08232288B2

反応ノート

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