Dimethylformamide → HCID 86696920、化合物

HRID 68545ノート

反応式

HRID 68545 の反応式
[C:1]1([N:7]2[C:12](=[O:13])[NH:11][C:10](=[O:14])[C:9]([C:15]#[N:16])=[N:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:17]N(C=O)C.[H-].[Na+].Br[CH2:25][CH:26]=[CH2:27]>O>[C:1]1([N:7]2[C:12](=[O:13])[N:11]([CH2:27][CH2:26][CH2:25][CH3:17])[C:10](=[O:14])[C:9]([C:15]#[N:16])=[N:8]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 7841Allyl bromideHCID 24758Sodium hydrideHCID 563387HCID 563387、化合物

生成物 1

HCID 86696920HCID 86696920、化合物収率 82%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Intermediate c (9 g, 0.042 mol) was added to DMF (80 mL) under an ice bath. To the mixture was added NaH (1.3 g, 0.054 mol) in batch under an ice bath. After stirring for 30 min, 3-bromopropylene (2.9 mL, 0.042 mol) was added dropwise. After the dropwise addition, the reaction was conducted at 50° C. for 4 h. After completion of the reaction, the reaction solution was poured into water (300 mL). A great deal of solid separated out and was filtered by suction. The filtered cake was washed with water and dried to produce Intermediate f (7.9 g) in a yield of 82%.

後処理

  1. additionAfter the dropwise addition
  2. waitthe reaction was conducted at 50° C. for 4 h
  3. customAfter completion of the reaction
  4. customA great deal of solid separated out
  5. filtrationwas filtered by suction
  6. washThe filtered cake was washed with water
  7. customdried

出典と根拠

ORDレコード
ord-e31211fd82754a77befa36a14160dfeb
出典データセット
uspto-grants-2014_09
特許番号
US08822465B2

反応ノート

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