Water → HCID 86734144、化合物

HRID 1729916ノート

反応式

HRID 1729916 の反応式
[H-].[Na+].[C:3]([O:6][CH:7]([CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])[CH2:8][CH2:9][CH2:10][NH:11][C:12]#[N:13])(=[O:5])[CH3:4].Br[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH:25]([CH3:31])[C:26]([O:28][CH2:29][CH3:30])=[O:27].O>C1C=CC=CC=1>[C:3]([O:6][CH:7]([CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])[CH2:8][CH2:9][CH2:10][N:11]([CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH:25]([CH3:31])[C:26]([O:28][CH2:29][CH3:30])=[O:27])[C:12]#[N:13])(=[O:5])[CH3:4]

参加物

6

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 215014751-(Cyanoamino)nonan-4-yl acetateHCID 22770549Ethyl 7-bromo-2-methylheptanoate

生成物 1

HCID 86734144HCID 86734144、化合物

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

実験手順

A stirred suspension of sodium hydride (57% in mineral oil) (5.0 g., excess) in a solvent mixture of benzene (75 ml.) and dimethylformide (75 ml.) is treated, over 30 minutes, with 4-acetoxynonylcyanamide (22.6 g., 0.1 mole) (Example O, Step 5) dissolved in benzene (20 ml.). Stirring is continued for one hour. Then, ethyl 7-bromo-2-methylheptanoate (Example L, Step 4) (25.3 g., 0.1 mole) is added dropwise, and the reaction is heated on the steam bath for 3.5 hours. The cooled reaction is poured into water (400 ml.) and extracted with ethyl acetate (2 × 200 ml.). The organic fractions are combined, washed with brine, then dried over sodium sulfate. The solvent is removed in vacuo to give ethyl 7-[N-(4-acetoxynonyl)cyanamido]-2-methylheptanoate as a pale yellow liquid.

後処理

  1. temperaturethe reaction is heated on the steam bath for 3.5 hours
  2. customThe cooled reaction
  3. extractionextracted with ethyl acetate (2 × 200 ml.)
  4. washwashed with brine
  5. dry with materialdried over sodium sulfate
  6. customThe solvent is removed in vacuo

出典と根拠

ORDレコード
ord-1741e1ff249d42b790b915bcb5f1312f
出典データセット
uspto-grants-1976_11
特許番号
US03989749

反応ノート

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