Triethylamine → HCID 15170720、化合物

HRID 486884

反応式

HRID 486884 の反応式
[SH:1][C:2]([CH3:13])([CH3:12])[C:3]([NH:5][C@H:6]([C:9](O)=[O:10])[CH2:7][SH:8])=[O:4].[CH:14]1([N:20]=[C:21]=NC2CCCCC2)CCCCC1.Cl.CNC.C(N(CC)CC)C>C(Cl)Cl.CO.C(OC(=O)C)C>[CH3:14][N:20]([CH3:21])[C:9](=[O:10])[C@H:6]([CH2:7][SH:8])[NH:5][C:3](=[O:4])[C:2]([SH:1])([CH3:13])[CH3:12]

参加物

8

反応物 4

HCID 8471TriethylamineHCID 10473Dimethylamine, hydrochlorideHCID 10868DicyclohexylcarbodiimideHCID 656604Bucillamine

生成物 1

HCID 15170720HCID 15170720、化合物収率 98.9%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒3 回HCID 8857Ethyl Acetate溶媒

実験手順

To a stirred solution of N-(2-mercapto-2-methylpropionyl)-L-cysteine (1.0 g) in methylene chloride(4 ml), dicyclohexylcarbodiimide (0.5 g) dissolved in methylene chloride(4 ml) was added dropwise. After the addition, the reaction mixture was stirred for 30 minutes under ice cooling and for 1 hour at room temperature. Dimethylamine hydrochloride(0.2 g) and triethylamine(0.4 ml) dissolved in a mixture of methylene chloride (2 ml) and methanol(1 ml) was added dropwise under ice-cooling. The reaction mixture was stirred for 15 minutes under ice-cooling and 3 hours at room temperature. To the reaction mixture, ethylacetate was added and filtered. The organic layer was washed with water and concentrated in vacuo. The oily residue was purified by a silica gel column chromatography to give 0.6 g(50%) of the titled compound.

後処理

  1. additionwas added dropwise
  2. additionAfter the addition
  3. additionwas added dropwise under ice-
  4. temperaturecooling
  5. stirringThe reaction mixture was stirred for 15 minutes under ice-
  6. temperaturecooling and 3 hours at room temperature
  7. filtrationfiltered
  8. washThe organic layer was washed with water
  9. concentrationconcentrated in vacuo
  10. customThe oily residue was purified by a silica gel column chromatography

出典と根拠

ORDレコード
ord-327165254db84b20a3c597fffea4a873
出典データセット
uspto-grants-1994_03
特許番号
US05292926

関連ノート

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