Triethylamine → 2-(methylthio)-N-(2-methylpent-3-yn-2-yl)acetamide

HRID 217155노트

반응식

HRID 217155 반응식
C(N([CH2:6][CH3:7])CC)C.Cl.[NH2:9][C:10]([CH3:15])([CH3:14])[C:11]#[C:12][CH3:13].CC[C:18](O)=[S:19].C1C=CC2N([OH:30])N=NC=2C=1>CN(C=O)C.O.C(Cl)CCl>[CH3:18][S:19][CH2:6][C:7]([NH:9][C:10]([CH3:15])([C:11]#[C:12][CH3:13])[CH3:14])=[O:30]

참가 물질

8

반응물 4

HCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 219231292-Methylpent-3-yn-2-amine hydrochlorideHCID 178460587HCID 178460587, 화합물

생성물 1

HCID 860149882-(methylthio)-N-(2-methylpent-3-yn-2-yl)acetamide

시약·촉매·용매 3

HCID 111,2-Dichloroethane용매HCID 962Water용매HCID 6228Dimethylformamide용매2회

실험 절차

Triethylamine (1.84 ml) was added to a stirred solution of 4-amino-4-methyl -pent-2-yne hydrochloride (1.278 g) in DMF (5 ml) at ambient temperature giving a white suspension. Methylthioacetic acid (1.0 g) was dissolved in DMF (5 ml) then added to the amine followed by HOBT (1.27 g) and finally EDC (1.806 g). The white suspension was stirred at room temperature for 6 hours and stored overnight. Water was added and the aqueous phase was extracted with diethyl ether. The organic phases were combined, successively washed with water and dried over magnesium sulphate, filtered and evaporated under reduced pressure to give 2-(methylthio)-N-(2-methylpent-3-yn -2-yl)acetamide as a yellow orange solid (1.9 g).

후처리

  1. customgiving a white suspension
  2. waitstored overnight
  3. extractionthe aqueous phase was extracted with diethyl ether
  4. washsuccessively washed with water
  5. dry with materialdried over magnesium sulphate
  6. filtrationfiltered
  7. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-3cb2954a609a4cd68295d3d763811755
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08193361B2

반응 노트

불러오는 중…