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Triethylamine → 1,2,4-Oxadiazole, 5-cyclopropyl-3-(isocyanomethyl)-

HRID 476867
ノート
印刷プレビュー

反応式

HRID 476867 の反応式
[CH:1]1([C:4]2[O:8][N:7]=[C:6]([CH2:9][NH:10][CH:11]=O)[N:5]=2)[CH2:3][CH2:2]1.C(N(CC)CC)C.O=P(Cl)(Cl)Cl.C([O-])([O-])=O.[Na+].[Na+]>C(Cl)Cl.O>[CH:1]1([C:4]2[O:8][N:7]=[C:6]([CH2:9][N+:10]#[C-:11])[N:5]=2)[CH2:3][CH2:2]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 8471TriethylamineHCID 10340Sodium CarbonateHCID 24813Phosphorus oxychlorideHCID 10749597HCID 10749597、化合物

生成物 1

HCID 107493421,2,4-Oxadiazole, 5-cyclopropyl-3-(isocyanomethyl)-

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6344
Dichloromethane
溶媒

実験手順

A stirred solution of 5-cyclopropyl-3-formylaminomethyl-1,2,4-oxadiazole (60 mmol) and triethylamine (176 mmol) in CH2Cl2 (100 ml) was charged dropwise with POCl3 (60 mmol) at 0° C. The mixture was then left for 30 min. with stirring at 0° C., whereafter a solution of Na2CO3 (60 mmol) in H2O (50 ml) was added. The mixture was heated to room temperature, whereafter the organic phase was separated, dried and evaporated in vacuo. The residue was treated with ether, decanted and the solution was evaporated to give the title compound as an oil. The oil was procssed without any further purification. The compound was characterized by its IR stretching band at 2160 cm-1.

後処理

  1. additionwas added
  2. customwas separated
  3. customdried
  4. customevaporated in vacuo
  5. additionThe residue was treated with ether
  6. customdecanted
  7. customthe solution was evaporated

出典と根拠

ORDレコード
ord-7e5f7b5dc8f345d4a40636a0c9b3560e
出典データセット
uspto-grants-1989_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04886797

反応ノート

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