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Water → HCID 18689504、化合物

HRID 1290142
ノート
印刷プレビュー

反応式

HRID 1290142 の反応式
O.[NH2:2][NH2:3].[Cl:4][C:5]1[C:6](F)=[N:7][C:8]([F:15])=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:10]=1.O>C(O)CC>[Cl:4][C:5]1[C:6]([NH:2][NH2:3])=[N:7][C:8]([F:15])=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:10]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 24654Hydrazine hydrate (1:1)HCID 11042190HCID 11042190、化合物

生成物 1

HCID 18689504HCID 18689504、化合物

試薬・触媒・溶媒 1

HCID 10311-Propanol溶媒

実験手順

10.5 g (0.21 mol) of hydrazine hydrate were added to a stirred mixture of 21.8 g (0.1 mol) of 3-chloro-2,6-difluoro-5-trifluoromethylpyridine in 100 ml of propanol at 50° C. in the course of 15 minutes, and stirring was continued for 2 hours at the same temperature. After cooling, the batch was poured into 1.5 l of water and the precipitate which had separated out was filtered off with suction. It was taken up in ethyl acetate for purification and extracted using water. After drying and concentration, 20.9 g (91% of theory) of the title compound of m.p. 104°-106° C. were obtained; a sublimated sample melted at 111°-113° C.

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. temperatureAfter cooling
  2. customthe precipitate which had separated out
  3. filtrationwas filtered off with suction
  4. customIt was taken up in ethyl acetate for purification
  5. extractionextracted
  6. customAfter drying
  7. concentrationconcentration, 20.9 g (91% of theory) of the title compound of m.p. 104°-106° C.
  8. customwere obtained

出典と根拠

ORDレコード
ord-e7a7a7690e4b4f419f09e90d469d0d25
出典データセット
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05750705

反応ノート

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