Ammonia → HCID 58709443、化合物

HRID 18675ノート

反応式

HRID 18675 の反応式
[NH3:1].[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]2[C:14](=[O:15])[CH:13]=[C:12]([C:16]([F:19])([F:18])[F:17])[N:11]([CH3:20])[C:10]2=[O:21])=[CH:5][C:4]=1[S:22](Cl)(=[O:24])=[O:23].C(OCC)(=O)C.Cl>O1CCCC1>[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]2[C:14](=[O:15])[CH:13]=[C:12]([C:16]([F:19])([F:18])[F:17])[N:11]([CH3:20])[C:10]2=[O:21])=[CH:5][C:4]=1[S:22]([NH2:1])(=[O:24])=[O:23]

参加物

6

反応物 4

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 153348022-chloro-5-(3,6-dihydro-3-methyl-4-trifluoromethyl-2,6-dioxo-1(2H)pyrimidinyl)benzenesulfonyl chloride

生成物 1

HCID 58709443HCID 58709443、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

With stirring, 1.6 g (93.8 mmol) of ammonia gas were, at 0° C., introduced into a mixture of 18 g (44.6 mmol) of 2-chloro-5-[3,6-dihydro-3-methyl-2,6-dioxo-4-trifluoromethyl-(2H)-pyrimidin-1-yl]-benzenesulfonylchloride in tetrahydrofuran (THF). Then, at 10° C., ethyl acetate was added and the mixture was acidified with 1N hydrochloric acid. The phases were separated and the aqueous phase was extracted, and the combined organic phases were then washed, dried and the solvent was removed. Customary purification methods gave 14.4 g (82.4% of theory) of the title compound (m.p.: 257-258° C.).

後処理

  1. customwere, at 0° C.
  2. customThe phases were separated
  3. extractionthe aqueous phase was extracted
  4. washthe combined organic phases were then washed
  5. customdried
  6. customthe solvent was removed
  7. customCustomary purification methods

出典と根拠

ORDレコード
ord-767ea4798cf34ce680042a650d7279d7
出典データセット
uspto-grants-2010_06
特許番号
US07741485B2

反応ノート

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