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

HRID 563887ノート

反応式

HRID 563887 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) giving a white suspension. Methylthioacetic acid (1.0 g) in DMF (5 ml) was then added to the amine followed by the HOBT (1.27 g) and finally EDC (1.806 g). The white suspension was stirred at ambient temperature for 6 hours, and stored for 18 hours. Water was added and the aqueous phase was extracted with diethyl ether. The organic phases were combined, washed with water and dried over magnesium sulphate then filtered and evaporated 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 for 18 hours
  3. extractionthe aqueous phase was extracted with diethyl ether
  4. washwashed with water
  5. dry with materialdried over magnesium sulphate
  6. filtrationthen filtered
  7. customevaporated

出典と根拠

ORDレコード
ord-ebacb50a592d4e359ac795237b12617b
出典データセット
uspto-grants-2011_11
特許番号
US08067592B2

反応ノート

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