Sulfuric Acid → HCID 23454145、化合物

HRID 1277480ノート

反応式

HRID 1277480 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][CH:19]([CH3:23])[CH2:20][CH2:21][CH3:22])[CH3:17].S(=O)(=O)(O)[OH:26]>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][CH:19]([CH3:23])[CH2:20][CH2:21][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

5

反応物 3

HCID 1118Sulfuric AcidHCID 345881N-(Cyanomethyl)-phthalimideHCID 5221872,4-Dimethylheptan-2-ol

生成物 1

HCID 23454145HCID 23454145、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

2-Phthalimidoacetonitrile (3.85 g) was dissolved in glacial acetic acid at 70° and 2,4-dimethylheptan-2-ol (3 g) was added; followed dropwise by conc. sulphuric acid (2.8 ml) the temperature being maintained between 65° and 70°. The final mixture was stirred for 15 minutes and then added slowly to ice cold water (150 ml). The resulting solid was collected, washed with water and dried in vacuo. It was dissolved in hot benzene, a little insoluble material filtered off and light petroleum (b.p. 40°-60° ) added to give 2-phthalimido-N-(1,1,3-trimethylhexyl)acetamide as a colourless solid, m.p. 131.6°.

後処理

  1. temperaturebeing maintained between 65° and 70°
  2. customThe resulting solid was collected
  3. washwashed with water
  4. customdried in vacuo
  5. dissolutionIt was dissolved in hot benzene
  6. filtrationa little insoluble material filtered off
  7. additionlight petroleum (b.p. 40°-60° ) added

出典と根拠

ORDレコード
ord-336a86f956ff426da5e66c4eb9c0ba39
出典データセット
uspto-grants-1981_07
特許番号
US04277498

反応ノート

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