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

HRID 217155ノート

反応式

HRID 217155 の反応式
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]

参加物

8

反応物 4

HCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 219231292-Methylpent-3-yn-2-amine hydrochlorideHCID 178460587HCID 178460587、化合物

生成物 1

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

試薬・触媒・溶媒 3

HCID 111,2-Dichloroethane溶媒HCID 962Water溶媒HCID 6228Dimethylformamide溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-3cb2954a609a4cd68295d3d763811755
出典データセット
uspto-grants-2012_06
特許番号
US08193361B2

反応ノート

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