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Dimethylformamide → HCID 178457084、化合物

HRID 240914
ノート
印刷プレビュー

反応式

HRID 240914 の反応式
C([O:8][C:9]1[CH:17]=[C:16]([O:18]CC2C=CC=CC=2)[C:15]([CH:26]([CH3:28])[CH3:27])=[CH:14][C:10]=1[C:11](O)=O)C1C=CC=CC=1.C(Cl)(=O)C(Cl)=O.C[N:36]([CH:38]=[O:39])C.[CH3:40][O:41][C:42]1[CH:47]=[CH:46][C:45]([NH2:48])=[CH:44][C:43]=1[N:49]([CH3:53])[CH2:50][CH2:51][CH3:52].C([N:56](CC)CC)C>ClCCl.C1COCC1.O.C(OCC)(=O)C>[OH:39][C:38]1[N:48]([C:45]2[CH:46]=[CH:47][C:42]([O:41][CH3:40])=[C:43]([N:49]([CH3:53])[CH2:50][CH2:51][CH3:52])[CH:44]=2)[C:11]([C:10]2[CH:14]=[C:15]([CH:26]([CH3:27])[CH3:28])[C:16]([OH:18])=[CH:17][C:9]=2[OH:8])=[N:56][N:36]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 5

HCID 6228DimethylformamideHCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 591678792,4-Dibenzyloxy-5-isopropyl-benzoic acidHCID 591678804-Methoxy-N3-methyl-N3-propyl-benzene-1,3-diamine

生成物 1

HCID 178457084HCID 178457084、化合物収率 93%

試薬・触媒・溶媒

4
HCID 962Water溶媒HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

2,4-Bis-benzyloxy-5-isopropylbenzoic acid (1.25 g, 3.32 mmol) was dissolved in dichloromethane (50 mL) and cooled in an ice bath. Oxalyl chloride (0.32 mL, 3.65 mmol) was added followed by the dropwise addition of DMF (0.1 mL). The reaction was stirred at room temperature for 1 hr then evaporated to dryness under reduced pressure to produce a brown solid. This solid was dissolved in THF (50 mL) and cooled in an ice bath. A solution of 4-Methoxy-N3-methyl-N3-propyl-benzene-1,3-diamine (0.71 g, 3.65 mmol) in THF (20 mL) was added dropwisely followed by the triethylamine (1.6 mL) and the reaction was stirred at room temperature for 16 hrs. Ethyl acetate (50 mL) and water (100 mL) were added. The ethyl acetate layer was washed with water (3×50 mL), dried over magnesium sulfate, filtered and evaporated to dryness to produce the crude product as a brown solid. Purification by silicagel chromatography (elution with 25% ethyl acetate/hexane) provided the desired compound as a white solid (1.8 g, 93%).

後処理

  1. temperaturecooled in an ice bath
  2. customthen evaporated to dryness under reduced pressure
  3. customto produce a brown solid
  4. temperaturecooled in an ice bath
  5. stirringthe reaction was stirred at room temperature for 16 hrs
  6. washThe ethyl acetate layer was washed with water (3×50 mL)
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltered
  9. customevaporated to dryness
  10. customto produce the crude product as a brown solid
  11. customPurification
  12. washby silicagel chromatography (elution with 25% ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-e647e0a13a4d48f384dbe7b4d115f67e
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08648104B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート