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

HRID 1277485

반응식

HRID 1277485 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
60 °C

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-a48c9c223f89431c8439d70714812a71
출처 데이터셋
uspto-grants-1981_07
특허 번호
US04277498

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