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Methanol → HCID 178478703、化合物

HRID 22935
ノート
印刷プレビュー

反応式

HRID 22935 の反応式
C(#N)C.CO.[Cl:6][CH2:7][C:8]([N:10]1[C@H:14]([C:15]#[N:16])[CH2:13][S:12][CH2:11]1)=[O:9].[N+:17]([C:20]1[CH:21]=[CH:22][C:23]([NH:26][C@H:27]2[CH2:32][CH2:31][C@H:30]([NH2:33])[CH2:29][CH2:28]2)=[N:24][CH:25]=1)([O-:19])=[O:18]>C(OCC)(=O)C.C(Cl)(Cl)Cl.CCOCC.O>[ClH:6].[ClH:6].[C:15]([C@@H:14]1[CH2:13][S:12][CH2:11][N:10]1[C:8](=[O:9])[CH2:7][NH:33][C@H:30]1[CH2:31][CH2:32][C@H:27]([NH:26][C:23]2[CH:22]=[CH:21][C:20]([N+:17]([O-:19])=[O:18])=[CH:25][N:24]=2)[CH2:28][CH2:29]1)#[N:16]
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 4

HCID 887MethanolHCID 6342AcetonitrileHCID 55265408(4R)-3-(chloroacetyl)-1,3-thiazolidine-4-carbonitrileHCID 178511612HCID 178511612、化合物

生成物 1

HCID 178478703HCID 178478703、化合物

試薬・触媒・溶媒 4

HCID 962Water溶媒
HCID 3283
Diethyl Ether
溶媒
HCID 6212Chloroform溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 2 ml of acetonitrile-1 ml of methanol containing 100 mg of (R)-3-chloroacetyl-4-cyanothiazolidine (the compound of Reference Example 2 mentioned below) and 372 mg of N-(5-nitro-2-pyridyl)-trans-1,4-cyclohexanediamine was stirred at room temperature for 15 hours. Water was added to the reaction mixture and the mixture was extracted with chloroform. After the extract was dried over anhydrous sodium sulfate, the solvent was removed under reduced pressure. The residue was purified by diol column chromatography (solvent: 0 to 5% methanol-chloroform) to obtain an oily product. The oily product was dissolved in 0.5 ml of ethyl acetate-0.5 ml of chloroform, and 1.0 ml of 2N hydrochloric acid-ether was added thereto, followed by 2 ml of ether. Precipitates were collected by filtration and washed with ether to obtain 173 mg of (R)-4-cyano-3-[trans-4-(5-nitro-2-pyridylamino)cyclohexylamino]acetylthiazolidine.dihydrochloride (Example 4-1 in Table 4).

後処理

  1. extractionthe mixture was extracted with chloroform
  2. dry with materialAfter the extract was dried over anhydrous sodium sulfate
  3. customthe solvent was removed under reduced pressure
  4. customThe residue was purified by diol column chromatography (solvent: 0 to 5% methanol-chloroform)
  5. customto obtain an oily product
  6. additionwas added
  7. customPrecipitates
  8. filtrationwere collected by filtration
  9. washwashed with ether

出典と根拠

ORDレコード
ord-c2eceec73ba2418f935e9c3c291606f9
出典データセット
uspto-grants-2005_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06849622B2

反応ノート

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