Ethyl cysteinate hydrochloride → HCID 14600711、化合物

HRID 1638989

反応式

HRID 1638989 の反応式
Cl.[CH2:2]([O:4][C:5](=[O:10])[C@H:6]([CH2:8][SH:9])[NH2:7])[CH3:3].[O-]CC.[Na+].[Na].[CH2:16]([O:23][C:24]([N:26]1[CH2:31][CH2:30][CH:29]([CH2:32][CH2:33]I)[CH2:28][CH2:27]1)=[O:25])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>C(O)C>[CH2:2]([O:4][C:5](=[O:10])[C@H:6]([CH2:8][S:9][CH2:33][CH2:32][CH:29]1[CH2:28][CH2:27][N:26]([C:24]([O:23][CH2:16][C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)=[O:25])[CH2:31][CH2:30]1)[NH2:7])[CH3:3]

参加物

6

反応物 4

HCID 2723617Ethyl cysteinate hydrochlorideHCID 2723922Sodium ethoxideHCID 5360545SodiumHCID 14600697Benzyl 4-(2-iodoethyl)piperidine-1-carboxylate

生成物 1

HCID 14600711HCID 14600711、化合物収率 92.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

In a nitrogen gas flow, 8.3 g of L-cysteine ethyl ester hydrochloride is added to a sodium ethoxide solution prepared by adding 2 g of metallic sodium to 80 ml of absolute ethanol. After stirring for 1 hours at room temperature, 80 ml of an ethanol solution containing 18.4 g of 2-(1-benzyloxycarbonyl-4-piperidyl)ethyl iodide is added dropwise to this reaction mixture. After stirring for 1 hour at room temperature, the reaction liquid is concentrated under reduced pressure. To the resulting residue, ice-cold water is added. After extracting with ether, the organic layer is washed with water, and dried over magnesium sulfate. Thereafter, the solvent is distilled off under reduced pressure to give 16.3 g of oily S-[2-(1-benzyloxycarbonyl-4-piperidyl)ethyl]-L-cysteine ethyl ester.

後処理

  1. customprepared
  2. additionis added dropwise to this reaction mixture
  3. stirringAfter stirring for 1 hour at room temperature
  4. customthe reaction liquid
  5. concentrationis concentrated under reduced pressure
  6. additionTo the resulting residue, ice-cold water is added
  7. extractionAfter extracting with ether
  8. washthe organic layer is washed with water
  9. dry with materialdried over magnesium sulfate
  10. distillationThereafter, the solvent is distilled off under reduced pressure

出典と根拠

ORDレコード
ord-c92e75a3332149228b45d799ac941ab9
出典データセット
uspto-grants-1989_11
特許番号
US04882326

関連ノート

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