Dimethylformamide → HCID 86696920、化合物

HRID 880047ノート

反応式

HRID 880047 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.CN(C=O)C.[H-].[Na+].[CH2:24](Br)[CH2:25][CH2:26][CH3:27]>O>[C:1]1([N:7]2[C:12](=[O:13])[N:11]([CH2:24][CH2:25][CH2:26][CH3:27])[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 8002Butyl bromideHCID 24758Sodium hydrideHCID 563387HCID 563387、化合物

生成物 1

HCID 86696920HCID 86696920、化合物収率 81.4%

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 (100 mL). To the mixture was added NaH (1.3 g, 0.054 mol) in batch under an ice bath. After stirring for 30 min, n-butyl bromide (3.4 mL, 0.042 mol) was added dropwise. Ater the dropwise addition, the reaction was conducted at 70° C. for 6 h. After completion of the reaction, the reaction solution was poured into water (600 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 (8.2 g) in a yield of 81.4%.

後処理

  1. additionAter the dropwise addition
  2. waitthe reaction was conducted at 70° C. for 6 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-028462de4cb6418981cbde3d311a603f
出典データセット
uspto-grants-2015_03
特許番号
US08993566B2

反応ノート

読み込み中…