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Water → 4-[4,4-Dimethyl 2,5-dioxo 3-(4-methoxybutyl) 1-imidazolidinyl] 2-(trifluoromethyl)-benzonitrile

HRID 355596
ノート
印刷プレビュー

反応式

HRID 355596 の反応式
[H-].[Na+].[CH3:3][C:4]1([CH3:28])[C:8](=[O:9])[N:7]([C:10]2[CH:17]=[CH:16][C:13]([C:14]#[N:15])=[C:12]([C:18]([F:21])([F:20])[F:19])[CH:11]=2)[C:6](=[O:22])[N:5]1[CH2:23][CH2:24][CH2:25][CH2:26][OH:27].[CH3:29]I.O>CN(C)C=O>[CH3:3][C:4]1([CH3:28])[C:8](=[O:9])[N:7]([C:10]2[CH:17]=[CH:16][C:13]([C:14]#[N:15])=[C:12]([C:18]([F:19])([F:20])[F:21])[CH:11]=2)[C:6](=[O:22])[N:5]1[CH2:23][CH2:24][CH2:25][CH2:26][O:27][CH3:29]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 6328Methyl iodide2 回HCID 24758Sodium hydride2 回HCID 1329814-(3-(4-Hydroxybutyl)-4,4-dimethyl-2,5-dioxo-1-imidazolidinyl)-2-(trifluoromethyl)benzonitrile

生成物 1

HCID 221169174-[4,4-Dimethyl 2,5-dioxo 3-(4-methoxybutyl) 1-imidazolidinyl] 2-(trifluoromethyl)-benzonitrile

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

50 mg of sodium hydride were added in several lots to 370 mg of the product of Example 58 in solution in 3 ml of dimethylformamide and the mixture was stirred for 20 minutes. 0.06 ml of methyl iodide were added and the mixture was stirred for one hour. A further 50 mg of sodium hydride were added and then after 20 minutes, 0.06 ml of methyl iodide were added. The reaction medium was poured into water and extracted with ether. The extracts were washed with water, dried and the solvent was evaporated. The residue was chromatographed on silica (eluant: methylene chloride--acetone 98-2) to obtain 135 mg of the expected product melting at 80°-81° C.

後処理

  1. stirringthe mixture was stirred for one hour
  2. waitafter 20 minutes
  3. extractionextracted with ether
  4. washThe extracts were washed with water
  5. customdried
  6. customthe solvent was evaporated
  7. customThe residue was chromatographed on silica (eluant: methylene chloride--acetone 98-2)

出典と根拠

ORDレコード
ord-c4190a384c3544f4a17c014e74f707bf
出典データセット
uspto-grants-1998_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
USRE035956

反応ノート

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