Water → 2-phthalimido-N-(1,1,5-trimethylhexyl)acetamide

HRID 1277485

反応式

HRID 1277485 の反応式
[C:1]1(=[O:14])[N:5]([CH2:6][C:7]#[N:8])[C:4](=[O:9])[C:3]2=[CH:10][CH:11]=[CH:12][CH:13]=[C:2]12.[CH3:15][C:16](O)([CH2:18][CH2:19][CH2:20][CH:21]([CH3:23])[CH3:22])[CH3:17].S(=O)(=O)(O)[OH:26].O>C(O)(=O)C>[C:4]1(=[O:9])[N:5]([CH2:6][C:7]([NH:8][C:16]([CH3:17])([CH3:15])[CH2:18][CH2:19][CH2:20][CH:21]([CH3:23])[CH3:22])=[O:26])[C:1](=[O:14])[C:2]2=[CH:13][CH:12]=[CH:11][CH:10]=[C:3]12

参加物

6

反応物 4

HCID 962WaterHCID 1118Sulfuric AcidHCID 832682,6-Dimethyl-2-heptanolHCID 345881N-(Cyanomethyl)-phthalimide

生成物 1

HCID 234541502-phthalimido-N-(1,1,5-trimethylhexyl)acetamide

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
60 °C

実験手順

A suspension of phthalimidoacetonitrile (6.01 g, 0.03 mole) in glacial acetic acid (16 ml) was heated to 60° C. with stirring; 2,6-dimethylheptan-2-ol (4.64 g, 0.03 mole) was then added followed dropwise by concentrated sulphuric acid (4.4 ml, 0.08 mole). The temperature rapidly rose to 20° and was controlled at this temperature during the addition. When the addition was complete the solution was stirred for 5 minutes and then added slowly to a mixture of ice and water (350 g). The precipitated solid was filtered off, washed thoroughly with water and dried in vacuo. The product was recrystallised from benzene with filtering to afford 2-phthalimido-N-(1,1,5-trimethylhexyl)acetamide, m.p. 162°-163°.

後処理

  1. customrapidly rose to 20°
  2. additionwas controlled at this temperature during the addition
  3. additionWhen the addition
  4. stirringwas stirred for 5 minutes
  5. filtrationThe precipitated solid was filtered off
  6. washwashed thoroughly with water
  7. customdried in vacuo
  8. customThe product was recrystallised from benzene
  9. filtrationwith filtering

出典と根拠

ORDレコード
ord-a48c9c223f89431c8439d70714812a71
出典データセット
uspto-grants-1981_07
特許番号
US04277498

関連ノート

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