Triethylamine → HCID 178448319, 화합물

HRID 1620758노트

반응식

HRID 1620758 반응식
Cl.[CH3:2][N:3]([CH3:11])[C:4](=[O:10])[C@@H:5]([CH:7]([CH3:9])[CH3:8])[NH2:6].C(N(CC)CC)C.S=[C:20]1[CH2:24][S:23][C:22](=[O:25])[NH:21]1>C(O)C>[CH3:2][N:3]([CH3:11])[C:4](=[O:10])[C@@H:5]([CH:7]([CH3:9])[CH3:8])[NH:6][C:20]1[CH2:24][S:23][C:22](=[O:25])[N:21]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 15395954-Sulfanylidene-1,3-thiazolidin-2-oneHCID 866789221422130-24-2

생성물 1

HCID 178448319HCID 178448319, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of the crude product (19.6 g) containing N,N-dimethyl-D-valinamide hydrochloride obtained in B) and triethylamine (44.0 g) in ethanol (150 mL) was added 4-thioxothiazolidin-2-one (14.4 g) at room temperature. The reaction mixture was stirred at room temperature for 3 hr, and the solvent was evaporated under reduced pressure. The obtained solid was suspended in THF, and the suspension was filtered through celite pad and silica gel pad. The filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (NH, ethyl acetate) to give the title compound (4.2 g).

후처리

  1. customthe solvent was evaporated under reduced pressure
  2. filtrationthe suspension was filtered through celite pad and silica gel pad
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customthe residue was purified by silica gel column chromatography (NH, ethyl acetate)

출처 및 근거

ORD 기록
ord-cd42e56bb169407fbec553bffa73211e
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08772277B2

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