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Hydrochloric Acid → HCID 1490650、化合物

HRID 616396
ノート
印刷プレビュー

反応式

HRID 616396 の反応式
[C:1]1(=[O:10])[O:9][C:6]([CH3:8])([CH3:7])[O:5][C:3](=[O:4])[CH2:2]1.C(N(CC)CC)C.[Cl:18][C:19]1[CH:20]=[C:21]([N:26]=[C:27]=[O:28])[CH:22]=[CH:23][C:24]=1[Cl:25].Cl>CS(C)=O.O>[CH3:7][C:6]1([CH3:8])[O:9][C:1](=[O:10])[C:2]([C:27](=[O:28])[NH:26][C:21]2[CH:22]=[CH:23][C:24]([Cl:25])=[C:19]([Cl:18])[CH:20]=2)=[C:3]([OH:4])[O:5]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 76073,4-Dichlorophenyl isocyanateHCID 8471TriethylamineHCID 162492,2-Dimethyl-1,3-dioxane-4,6-dione

生成物 1

HCID 1490650HCID 1490650、化合物

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒2 回
HCID 962
Water
溶媒

実験手順

To a solution of 14.4 g of isopropylidene malonate in 150 ml of dimethyl sulphoxide were added dropwise, at room temperature, 10.1 g of triethylamine and thereafter, at 20° to 30° C, 18.8 g of 3,4-dichlorophenylisocyanate in 30 ml of dimethyl sulphoxide. The mixture was reacted for 12 to 15 hours at room temperature and the resultant solution was poured into a solution of 20 ml of concentrated hydrochloric acid in 200 ml of water. The precipitate which formed was collected with suction. Recrystallisation from 130 ml of acetone yielded the product of the formula ##STR5## with a melting point of 132°-134° C.

後処理

  1. customat 20° to 30° C
  2. customThe mixture was reacted for 12 to 15 hours at room temperature
  3. customThe precipitate which formed
  4. customwas collected with suction
  5. customRecrystallisation from 130 ml of acetone
  6. customyielded the product of the formula ##STR5## with a melting point of 132°-134° C.

出典と根拠

ORDレコード
ord-182466c2282648d3a5461bcd894e5c10
出典データセット
uspto-grants-1978_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04073932

反応ノート

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