N-(5,7-dichloro-2,3-dihydrobenzofuran-2-ylmethyl)-N-butylcarbamyl chloride → 1-(N-(5,7-dichloro-2,3-dihydrobenzofuran-2-ylmethyl)-N-butylcarbamyl)-1,2,4-triazole

HRID 1248931ノート

反応式

HRID 1248931 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([Cl:20])[C:5]2[O:9][CH:8]([CH2:10][N:11]([CH2:15][CH2:16][CH2:17][CH3:18])[C:12](Cl)=[O:13])[CH2:7][C:6]=2[CH:19]=1.[NH:21]1[CH:25]=[N:24][C-:23]=[N:22]1.[Na+]>O1CCCC1>[Cl:1][C:2]1[CH:3]=[C:4]([Cl:20])[C:5]2[O:9][CH:8]([CH2:10][N:11]([CH2:15][CH2:16][CH2:17][CH3:18])[C:12]([N:21]3[CH:25]=[N:24][CH:23]=[N:22]3)=[O:13])[CH2:7][C:6]=2[CH:19]=1

参加物

4

反応物 2

HCID 13563317N-(5,7-dichloro-2,3-dihydrobenzofuran-2-ylmethyl)-N-butylcarbamyl chlorideHCID 547199651,2,4-Triazolylsodium

生成物 1

HCID 135633191-(N-(5,7-dichloro-2,3-dihydrobenzofuran-2-ylmethyl)-N-butylcarbamyl)-1,2,4-triazole収率 88.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
65 °C

実験手順

13.5 g (0.04 mole) of N-(5,7-dichloro-2,3-dihydrobenzofuran-2-ylmethyl)-N-butylcarbamyl chloride were added dropwise to a suspension of 5.5 g (0.06 mole) of sodium 1,2,4-triazolide in 120 ml of dry tetrahydrofuran at 20° C. The mixture was stirred for 6 hours at 65° C., after which it was cooled to 20° C., and the precipitate was filtered off under suction. The filtrate was evaporated down, the residue was suspended in 30 ml of diethyl ether, and the product was filtered off under suction. 13.1 g of 1-(N-(5,7-dichloro-2,3-dihydrobenzofuran-2-ylmethyl)-N-butylcarbamyl)-1,2,4-triazole were obtained as colorless crystals of melting point 122°-124° C. (compound NO. 2).

後処理

  1. temperatureafter which it was cooled to 20° C.
  2. filtrationthe precipitate was filtered off under suction
  3. customThe filtrate was evaporated down
  4. filtrationthe product was filtered off under suction

出典と根拠

ORDレコード
ord-93532d0c347b4f2fa44558b967e4ab14
出典データセット
uspto-grants-1986_12
特許番号
US04628058

反応ノート

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