Hydrochloric Acid → HCID 178501253、化合物

HRID 2109048

反応式

HRID 2109048 の反応式
Cl.[NH2:2][C@H:3]1[CH2:8][CH2:7][C@H:6]([C:9]([O:11][CH3:12])=[O:10])[CH2:5][CH2:4]1.C(N(CC)CC)C.[Cl:20][CH2:21][CH2:22][CH2:23][S:24](Cl)(=[O:26])=[O:25].Cl>C(Cl)(Cl)Cl>[Cl:20][CH2:21][CH2:22][CH2:23][S:24]([NH:2][C@H:3]1[CH2:4][CH2:5][C@H:6]([C:9]([O:11][CH3:12])=[O:10])[CH2:7][CH2:8]1)(=[O:26])=[O:25]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 154103-Chloropropanesulphonyl chlorideHCID 178501210HCID 178501210、化合物

生成物 1

HCID 178501253HCID 178501253、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

Methyl trans-4-aminocyclohexanecarboxylate hydrochloride (4.08 g) obtained in Reference Example 2(1) is suspended in chloroform (50 ml), and thereto is added triethylamine (8.8 ml) under ice-cooling. Subsequently, a solution of 3-chloropropanesulfonyl chloride (3.35 ml) in chloroform (20 ml) is added dropwise over 20 minutes under the same temperature. After stirring for 2 hours at room temperature, 5% hydrochloric acid is added to the reaction solution and the mixture is extracted with chloroform. The organic layer is washed with saturated brine, dried over sodium sulfate and evaporated to remove the solvent under reduced pressure. The resulting residue is suspended in diisopropylamine, and filtered to collect precipitates to give methyl trans-4-{[(3-chloropropyl)sulfonyl]amino}cyclohexanecarboxylate (6.14 g).

後処理

  1. temperaturecooling
  2. extractionthe mixture is extracted with chloroform
  3. washThe organic layer is washed with saturated brine
  4. dry with materialdried over sodium sulfate
  5. customevaporated
  6. customto remove the solvent under reduced pressure
  7. filtrationfiltered
  8. customto collect
  9. customprecipitates

出典と根拠

ORDレコード
ord-b10aff07f00c45cfaf62bfa6e7fa0020
出典データセット
uspto-grants-2009_04
特許番号
US07514449B2

関連ノート

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