Diethyl Ether → HCID 86613736、化合物

HRID 40458

反応式

HRID 40458 の反応式
[CH2:1]([NH2:4])[CH2:2][NH2:3].C(N(CC)CC)C.[F:12][C:13]1[C:18]([C:19](Cl)=[O:20])=[C:17]([F:22])[C:16]([F:23])=[C:15]([F:24])[C:14]=1[F:25].CC[O:28]CC>>[F:12][C:13]1[C:18]([C:19]([OH:28])=[O:20])=[C:17]([F:22])[C:16]([F:23])=[C:15]([F:24])[C:14]=1[F:25].[F:12][C:13]1[C:18]([C:19]([OH:28])=[O:20])=[C:17]([F:22])[C:16]([F:23])=[C:15]([F:24])[C:14]=1[F:25].[CH2:1]([NH2:4])[CH2:2][NH2:3]

参加物

5

反応物 4

HCID 3283Diethyl Ether2 回HCID 3301EthylenediamineHCID 8471TriethylamineHCID 75256Pentafluorobenzoyl chloride

生成物 1

HCID 86613736HCID 86613736、化合物

実験手順

Ethylene diamine (130 mg, 2.1 mmol) and triethylamine (510 mg, 5.0 mmol), together dissolved in 10 mL anhydrous ether is added to pentafluorobenzoyl chloride (1.2 g, 5.0 mmol) in 10 mL anhydrous ether. White precipitate is obtained and filtered off. The residue is washed with chloroform, then water and then filtered to recover ethylene diamine bis(pentafluorobenzoate) (III) as white needle crystals (yield, 100%). Sodium azide (270 mg, 4.2 mmol) in 1.7 mL water and 4.0 mL DMF is then reacted with III (870 mg, 2.0 mmol) in 20 mL DMF, and stirred overnight on a 60° C. hotplate. A white precipitate is obtained. The solution is reduced to half-volume by evaporation and the precipitate is filtered off (yield, 35%), dried and recrystallised from DMF to give ethylene diamine bis(4-azido-2,3,5,6-tetrafluorobenzoate) (IV) as white crystals. FTIR: 2129 (N3 asymmetric stretch), 1666 (C═O stretch), 1554, 1483, 1242 (N3 symmetric stretch), no acid OH band at 3000-3500.

後処理

  1. customWhite precipitate is obtained
  2. filtrationfiltered off
  3. washThe residue is washed with chloroform
  4. filtrationwater and then filtered
  5. customto recover

出典と根拠

ORDレコード
ord-133a7ea9ff03486ea4b88148682a818d
出典データセット
uspto-grants-2013_09
特許番号
US08530269B2

関連ノート

読み込み中…