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Hydrochloric Acid → HCID 11234930、化合物

HRID 1791030
ノート
印刷プレビュー

反応式

HRID 1791030 の反応式
C[Si]([N-][Si](C)(C)C)(C)C.[Li+].[CH2:11]=[C:12]1[CH2:18][CH:17]([S:19]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)(=[O:21])=[O:20])[C:16]2[CH:28]=[C:29]([C:32]([O:34][CH3:35])=[O:33])[CH:30]=[CH:31][C:15]=2[O:14][CH2:13]1.[CH2:36](Br)[CH:37]=[CH2:38].Cl>O1CCCC1.ClCCl.O>[CH2:38]([C:17]1([S:19]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)(=[O:21])=[O:20])[C:16]2[CH:28]=[C:29]([C:32]([O:34][CH3:35])=[O:33])[CH:30]=[CH:31][C:15]=2[O:14][CH2:13][C:12](=[CH2:11])[CH2:18]1)[CH:37]=[CH2:36]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 7841Allyl bromideHCID 2733832Lithium hexamethyldisilazaneHCID 11439769HCID 11439769、化合物

生成物 1

HCID 11234930HCID 11234930、化合物収率 67%

試薬・触媒・溶媒 3

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

実験手順

0.023 ml (1.1 equivalents) of 1,3-dimethylpropyleneurea and then 0.189 ml (1.1 equivalents) of 1.06M lithium bis(trimethylsilyl)amide in tetrahydrofuran are added at ambient temperature to 61 mg (0.17 mmol) of methyl 3-methylene-5-(phenylsulfonyl)-2,3,4,5-tetrahydro-1-benzoxepin-7-carboxylate, prepared according to example 1, in solution in 1.8 ml of tetrahydrofuran. The reaction medium then assumes a dark yellow color. After stirring for 15 minutes, 0.0165 ml (1.1 equivalents) of allyl 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 25/55) to give 51 mg (67%) of methyl 5-allyl-3-methylene-5-(phenylsulfonyl)-2,3,4,5-tetrahydro-1-benzoxepin-7-carboxylate in the form of an oil; 1H NMR (300 MHz, CDCl3): 3.25 (m, 4H), 3.9 (s, 3H), 4.25 (d, J=14.3 Hz, 1H), 4.6 (d, J=14.3 Hz, 1H), 4.93 (s, 1H), 5.10 (s, 1H), 5.21 (m, 2H), 5.83 (m, 1H), 6.86 (d, J=8.5 Hz, 1H), 7.4 (m, 4H), 7.57 (m, 1H), 7.95 (dd, J=8.46 and 2 Hz, 1H), 8.21 (d, J=2.07 Hz, 1H).

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 25/55)

出典と根拠

ORDレコード
ord-fc1f3eb907b64e0188308cae0d70581a
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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