Triethylamine → HCID 15170720, 화합물

HRID 486884

반응식

HRID 486884 반응식
[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]

참가 물질

8

반응물 4

HCID 8471TriethylamineHCID 10473Dimethylamine, hydrochlorideHCID 10868DicyclohexylcarbodiimideHCID 656604Bucillamine

생성물 1

HCID 15170720HCID 15170720, 화합물수율 98.9%

시약·촉매·용매 3

HCID 887Methanol용매HCID 6344Dichloromethane용매3회HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-327165254db84b20a3c597fffea4a873
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05292926

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