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Sodium hydrosulfide → HCID 178499044、化合物

HRID 973831
ノート
印刷プレビュー

反応式

HRID 973831 の反応式
Cl[C:2]1[N:7]2[N:8]=[C:9]([C:11]([O:13][CH3:14])=[O:12])[N:10]=[C:6]2[N:5]=[C:4]([CH:15]([CH3:17])[CH3:16])[CH:3]=1.[SH-:18].[Na+]>O>[CH:15]([C:4]1[CH:3]=[C:2]([SH:18])[N:7]2[N:8]=[C:9]([C:11]([O:13][CH3:14])=[O:12])[N:10]=[C:6]2[N:5]=1)([CH3:17])[CH3:16]
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 28015Sodium hydrosulfideHCID 16767691Methyl 7-chloro-5-(propan-2-yl)-(1,2,4)triazolo(1,5-a)pyrimidine-2-carboxylate

生成物 1

HCID 178499044HCID 178499044、化合物収率 90.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

The product obtained in Step 2 (40 g) was added at 0° C. to a solution of sodium hydrosulfide (40 g) in one liter of water with stirring under a nitrogen stream. The mixture was stirred at 0° C. for one hour, then at room temperature for three hours, and the resulting yellow solution was washed with 200 ml of ethyl acetate. The aqueous layer was acidified with concentrated hydrochloric acid to pH 2.0, and the formed crystals were collected by filtration and washed with 100 ml of ethanol, affording 36 g of the objective compound as faint yellow crystals.

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

後処理

  1. stirringThe mixture was stirred at 0° C. for one hour
  2. washthe resulting yellow solution was washed with 200 ml of ethyl acetate
  3. filtrationthe formed crystals were collected by filtration
  4. washwashed with 100 ml of ethanol

出典と根拠

ORDレコード
ord-d865621457e049aca3126a068a0cb194
出典データセット
uspto-grants-1991_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05064953

反応ノート

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