Lithium Hydroxide → HCID 2800115、化合物

HRID 444460ノート

反応式

HRID 444460 の反応式
Cl[C:2]1[N:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][CH:3]=1.[Cl:11][C:12]1[CH:17]=[CH:16][C:15]([SH:18])=[CH:14][CH:13]=1.[OH-].[Li+]>CN(C=O)C>[Cl:11][C:12]1[CH:17]=[CH:16][C:15]([S:18][C:2]2[N:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][CH:3]=2)=[CH:14][CH:13]=1

参加物

5

実験手順

6-Chloro-3-nitropyridine (4.0 grams) and 4-chlorothiophenol (3.7 grams) were mixed in 100 ml. of dry DMF and lithium hydroxide (1.2 grams) added portionwise. After the reaction mixture had stirred for about 5 minutes, it darkened and became warm. It was allowed to stir with a drying tube for 4 hours, poured over ice water and the product separated by filtration. It was crystallized from ethyl acetate-ethanol, yield: 5.0 grams, m.p. 134°-136° C.

後処理

  1. temperaturebecame warm
  2. stirringto stir with a drying tube for 4 hours
  3. customthe product separated by filtration
  4. customIt was crystallized from ethyl acetate-ethanol, yield: 5.0 grams, m.p. 134°-136° C.

出典と根拠

ORDレコード
ord-57955474b9ae4295a26ab436bd0a52c1
出典データセット
uspto-grants-1981_04
特許番号
US04264605

反応ノート

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