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Bicarbonate Ion → HCID 57567638、化合物

HRID 883700
ノート
印刷プレビュー

反応式

HRID 883700 の反応式
Cl([O-])(=O)(=O)=O.[Li+].[NH2:7][CH2:8][CH2:9][N:10]1[C:14]2[CH:15]=[CH:16][C:17]([C:19]([N:21]([CH2:26][CH:27]([CH3:29])[CH3:28])[CH2:22][CH:23]([CH3:25])[CH3:24])=[O:20])=[CH:18][C:13]=2[N:12]=[C:11]1[NH:30][C:31]1[CH:36]=[C:35]([O:37][CH3:38])[C:34]([O:39][CH3:40])=[C:33]([O:41][CH3:42])[CH:32]=1.[O:43]1C[CH:44]1[CH2:45][C:46]1[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=1.C(=O)([O-])O>C(#N)C.ClCCl>[OH:43][CH:44]([NH:7][CH2:8][CH2:9][N:10]1[C:14]2[CH:15]=[CH:16][C:17]([C:19]([N:21]([CH2:22][CH:23]([CH3:25])[CH3:24])[CH2:26][CH:27]([CH3:28])[CH3:29])=[O:20])=[CH:18][C:13]=2[N:12]=[C:11]1[NH:30][C:31]1[CH:36]=[C:35]([O:37][CH3:38])[C:34]([O:39][CH3:40])=[C:33]([O:41][CH3:42])[CH:32]=1)[CH2:45][C:46]1[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 769Bicarbonate IonHCID 948262-(Phenylmethyl)oxiraneHCID 23665649Lithium perchlorateHCID 69027345HCID 69027345、化合物

生成物 1

HCID 57567638HCID 57567638、化合物

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒
HCID 6344
Dichloromethane
溶媒

実験手順

Lithium perchlorate (16 mg, 3 eq) then after 5 minutes 1-(2-aminoethyl)-N,N-diisobutyl-2-[(3,4,5-trimethoxy phenyl)amino]-1H-benzimidazole-5-carboxamide (25 mg, 1 eq) are added, at a temperature of approximately 20° C. to a solution of 2,3-epoxypropylbenzene (7 mg, 1 eq) in acetonitrile (0.5 ml). The mixture is heated under reflux for 24 hours then cooled down to ambient temperature and hydrogen carbonate and dichloromethane saturated water is added. After decanting and extracting, the organic phases are combined and washed with salt water, followed by drying over sodium sulphate and evaporating under reduced pressure at 40° C. Purification of the oil obtained by flash chromatography on silica gel (100% dichloromethane to dichloromethane/methanol 80:20) produces the expected compound in the form of an oil (31 mg, 55% yield)

後処理

  1. temperatureThe mixture is heated
  2. temperatureunder reflux for 24 hours
  3. customAfter decanting
  4. extractionextracting
  5. washwashed with salt water
  6. dry with materialby drying over sodium sulphate
  7. customevaporating under reduced pressure at 40° C
  8. customPurification of the oil
  9. customobtained by flash chromatography on silica gel (100% dichloromethane to dichloromethane/methanol 80:20)

出典と根拠

ORDレコード
ord-a0d8995e46f941f18196f0e0ba939898
出典データセット
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08236965B2

反応ノート

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