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Hydrochloric Acid → HCID 11362878、化合物

HRID 1791028
ノート
印刷プレビュー

反応式

HRID 1791028 の反応式
CN1CCCN(C)C1=O.C[Si]([N-][Si](C)(C)C)(C)C.[Li+].[CH2:20]=[C:21]1[CH2:27][CH:26]([S:28]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)(=[O:30])=[O:29])[C:25]2[CH:37]=[C:38]([C:41]([O:43][CH3:44])=[O:42])[CH:39]=[CH:40][C:24]=2[O:23][CH2:22]1.[CH2:45](Br)[C:46]1[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=1.Cl>O1CCCC1.ClCCl.O>[CH2:45]([C:26]1([S:28]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)(=[O:30])=[O:29])[C:25]2[CH:37]=[C:38]([C:41]([O:43][CH3:44])=[O:42])[CH:39]=[CH:40][C:24]=2[O:23][CH2:22][C:21](=[CH2:20])[CH2:27]1)[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

9

反応物 5

HCID 313Hydrochloric AcidHCID 7498Benzyl BromideHCID 816462(1H)-Pyrimidinone, tetrahydro-1,3-dimethyl-HCID 2733832Lithium hexamethyldisilazaneHCID 11439769HCID 11439769、化合物

生成物 1

HCID 11362878HCID 11362878、化合物収率 86%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

0.072 ml (1.1 equivalents) of 1,3-dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone and then 0.6 ml (1.1 equivalents) of 1.06M lithium bis(trimethylsilyl)amide in tetrahydrofuran are added at ambient temperature to 195 mg (0.55 mmol) of methyl 3-methylene-5-(phenylsulfonyl)-2,3,4,5-tetrahydro-1-benzoxepin-7-carboxylate, prepared according to example 1, in solution in 5 ml of tetrahydrofuran. The reaction medium then assumes a dark yellow color. After stirring for 15 minutes, 0.073 ml (1.1 equivalents) of benzyl bromide is added. After stirring for 5 minutes, water, 1N hydrochloric acid and dichloromethane are added. After separating the organic and aqueous phases, the aqueous phase is extracted three times with dichloromethane. The combined organic phases are washed with brine, are dried and are finally concentrated under vacuum. The crude reaction product is then purified by chromatography on silica gel (ethyl acetate/heptane 25/75) to provide 211 mg (86%) of methyl 5-benzyl-3-methylene-5-(phenylsulfonyl)-2,3,4,5-tetrahydro-1-benzoxepin-7-carboxylate in the form of a white solid; M.p.=164–165° C.

後処理

  1. customprepared
  2. stirringAfter stirring for 5 minutes
  3. customAfter separating the organic and aqueous phases
  4. extractionthe aqueous phase is extracted three times with dichloromethane
  5. washThe combined organic phases are washed with brine
  6. customare dried
  7. concentrationare finally concentrated under vacuum
  8. customThe crude reaction product
  9. customis then purified by chromatography on silica gel (ethyl acetate/heptane 25/75)

出典と根拠

ORDレコード
ord-8e1a81dcc4f34c74882563a072dc0774
出典データセット
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07071340B2

反応ノート

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