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1,3-Propanediamine → HCID 178526631、化合物

HRID 1628474
ノート
印刷プレビュー

反応式

HRID 1628474 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[N:11]=[C:12](Cl)Cl.[CH2:15]([NH2:19])[CH2:16][CH2:17][NH2:18]>O1CCCC1>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[N:11]=[C:12]1[NH:19][CH2:15][CH2:16][CH2:17][NH:18]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 4281,3-PropanediamineHCID 86632875(2-Chloro-5-nitrophenyl)carbonimidic dichloride

生成物 1

HCID 178526631HCID 178526631、化合物収率 98.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
7.5 °C

実験手順

(2-Chloro-5-nitrophenyl)carbonimidic dichloride (35.5 g, 140 mmol) was dissolved in tetrahydrofuran (135 mL). The solution was added dropwise within 30 min to a solution of 1,3-propanediamine (58 mL, 700 mmol) in tetrahydrofuran (335 mL) which was kept at 5-10° C. The reaction mixture was stirred for 1 h at 5-10° C. another 2 hr at room temperature. The suspension was filtered, and washed with tetrahydrofuran. The filtrate was concentrated in vacuo. The residue was taken up in water, filtered, and washed with water and diisopropyl ether. After drying at 50° C. under vacuum, the title compound (35.0 g, 137.4 mmol, 98%) was obtained as yellow crystals.

後処理

  1. customwas kept at 5-10° C
  2. filtrationThe suspension was filtered
  3. washwashed with tetrahydrofuran
  4. concentrationThe filtrate was concentrated in vacuo
  5. filtrationfiltered
  6. washwashed with water and diisopropyl ether
  7. customAfter drying at 50° C. under vacuum

出典と根拠

ORDレコード
ord-fbdc7aab0f1542e282d1cda170c6c9f5
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08785460B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート