Ethyl trifluoroacetate → HCID 20322683、化合物

HRID 2072213ノート

反応式

HRID 2072213 の反応式
FC(F)(F)C(OCC)=O.O.NN.[Cl:13][C:14]1[CH:19]=[CH:18][C:17]([N:20]=[C:21](Cl)[C:22]2[CH:27]=[CH:26][C:25]([Cl:28])=[CH:24][CH:23]=2)=[CH:16][CH:15]=1.[F:30][C:31]([F:38])([F:37])[C:32]1[NH:36][N:35]=CN=1>CO>[Cl:28][C:25]1[CH:26]=[CH:27][C:22]([C:21]2[N:20]([C:17]3[CH:18]=[CH:19][C:14]([Cl:13])=[CH:15][CH:16]=3)[C:32]([C:31]([F:38])([F:37])[F:30])=[N:36][N:35]=2)=[CH:23][CH:24]=1

参加物

6

反応物 4

HCID 9794Ethyl trifluoroacetateHCID 24654Hydrazine hydrate (1:1)HCID 12293810HCID 12293810、化合物HCID 189440113-(trifluoromethyl)-1H-1,2,4-triazole(SALTDATA: FREE)

生成物 1

HCID 20322683HCID 20322683、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Ethyl trifluoroacetate (2.9 g) was added to hydrazine hydrate (1.1 g, 99-100%) in methanol (20 ml) at 5°-10° and stirred for 15 min. N-(4-chlorophenyl)-4-chlorobenzimidoyl chloride (5.7 g) was added keeping the temperature below 5°for 3 hr and then at reflux for 1 hr 3,4bis 4-chlorophenyl)-5-trifluoromethyl-1,2,4-triazole crystallized on cooling (4.1 g, 57.8%) m.p. 184°. (Found: C, 50.54%; H, 2.40%; Cl, 19.6%; F, 15.8%; N, 11.54%. C15H8Cl2F3N3 requires: C, 50.30%; H, 2.25%; Cl, 19.8%; F, 15.9%; N, 11.73%) δ (CDCl3); 7.43 (m).

後処理

  1. custombelow 5°for 3 hr
  2. customcrystallized
  3. temperatureon cooling (4.1 g, 57.8%) m.p. 184°

出典と根拠

ORDレコード
ord-80fe19de265845c2bf39823ba133a118
出典データセット
uspto-grants-1977_09
特許番号
US04049815

反応ノート

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