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Dimethylamine → HCID 28165234, 화합물

HRID 2172686
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HRID 2172686 반응식
[C:1]([O:5][C:6]([NH:8][C@H:9]([CH3:13])[C:10](O)=[O:11])=[O:7])([CH3:4])([CH3:3])[CH3:2].C1CC[CH:17]([N:20]=[C:21]=NC2CCCCC2)CC1.CNC>C(Cl)Cl>[C:1]([O:5][C:6](=[O:7])[NH:8][C@@H:9]([C:10](=[O:11])[N:20]([CH3:21])[CH3:17])[CH3:13])([CH3:4])([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 674DimethylamineHCID 10868DicyclohexylcarbodiimideHCID 637606BOC-D-alanine

생성물 1

HCID 28165234HCID 28165234, 화합물수율 76%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of (R)-2-tert-Butoxycarbonylamino-propionic acid (1.78 g, 9.43 mmol) in DCM (7.85 mL) was added portion wise DCC (2.14 g, 10.37 mmol) cooled in an ice bath. After stirring at room temperature for 30 min, dimethylamine (2 M in THF) (6.13 mL, 12.25 mmol) was added. The resulting solution was stirred overnight (18 h) until reaction was completed. The reaction mixture was filtered through silica gel and eluted with Ethyl acetate. Then the filtrate was evaporated off. The solvent was removed to yield (1.71 g, 7.12 mmol, 76% yield, 90% purity) ((R)-1-Dimethylcarbamoyl-ethyl)-carbamic acid tert-butyl ester as a yellow oil. The product was used in the next step without further purification.

후처리

  1. temperaturecooled in an ice bath
  2. stirringThe resulting solution was stirred overnight (18 h)
  3. customuntil reaction
  4. filtrationThe reaction mixture was filtered through silica gel
  5. washeluted with Ethyl acetate
  6. customThen the filtrate was evaporated off
  7. customThe solvent was removed

출처 및 근거

ORD 기록
ord-11e319770c644f299b9baba76b30b38f
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09056843B2

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