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Putrescine → HCID 178526630、化合物

HRID 1628472
ノート
印刷プレビュー

反応式

HRID 1628472 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]([NH2:20])[CH2:16][CH2:17][CH2:18][NH2:19]>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:20][CH2:15][CH2:16][CH2:17][CH2:18][NH:19]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 1045PutrescineHCID 86632875(2-Chloro-5-nitrophenyl)carbonimidic dichloride

生成物 1

HCID 178526630HCID 178526630、化合物収率 48%

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 (17.8 g, 70.0 mmol) was dissolved in tetrahydrofuran (68 mL). The solution was added dropwise within 30 min to a solution of 1,4-butanediamine (30.9 g, 350 mmol) in tetrahydrofuran (168 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 disopropyl ether. After drying at 50° C. under vacuum, the title compound (8.9 g, 33.4 mmol, 48%) was obtained as a yellow amorphous.

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 disopropyl ether
  7. customAfter drying at 50° C. under vacuum

出典と根拠

ORDレコード
ord-7c27607417e64644b6c4df25daa4c4b6
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