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Diethylamine → HCID 54401837、化合物

HRID 436764
ノート
印刷プレビュー

反応式

HRID 436764 の反応式
[CH2:1]([NH:3][CH2:4][CH3:5])[CH3:2].[N:6]([C:15]([N:19]=[C:20]=[O:21])([CH2:17][CH3:18])[CH3:16])=[N:7][C:8]([N:12]=[C:13]=[O:14])([CH2:10][CH3:11])[CH3:9]>CCCCC>[N:6]([C:15]([NH:19][C:20]([N:3]([CH2:4][CH3:5])[CH2:1][CH3:2])=[O:21])([CH2:17][CH3:18])[CH3:16])=[N:7][C:8]([NH:12][C:13]([N:3]([CH2:4][CH3:5])[CH2:1][CH3:2])=[O:14])([CH2:10][CH3:11])[CH3:9]
参加物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 8021DiethylamineHCID 53785527HCID 53785527、化合物

生成物 1

HCID 54401837HCID 54401837、化合物

試薬・触媒・溶媒 1

HCID 8003Pentane溶媒

実験手順

To a stirred solution of 3.95 grams (0.054 moles) of diethylamine in 30 ml pentane in a 50 ml erlenmeyer flask cooled in a water bath was added 6.05 grams (0.027 moles) of 2,2'-azobis(2-isocyanatobutane) (from Example XXXVI) dropwise over 20 minutes while holding the reaction temperature below 30° C. After the addition was complete, the reaction was stirred for an additional 60 minutes at room temperature and filtered. The filter cake was washed with pentane and dried. The dry white solid weighed 1.8 grams (18% crude yield) and melted at 215°-220° C. with decomposition. The product had a broad carbonyl band at 1650 cm-1 and a strong NH band at 3400 cm-1 in its infrared spectrum and the isocyanate band at 2200 cm-1 was absent.

後処理

  1. customthe reaction temperature below 30° C
  2. additionAfter the addition
  3. filtrationfiltered
  4. washThe filter cake was washed with pentane
  5. customdried

出典と根拠

ORDレコード
ord-cb619d25a1e9480883de60b0b1bf8d5c
出典データセット
uspto-grants-1977_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04028344

反応ノート

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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