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Ammonia → 5-[3,6-Dihydro-3-methyl-2,6-dioxo-4-(trifluoromethyl)-1(2H)-pyrimidinyl]-1,2-benzisothiazole-3-acetamide

HRID 1274599
ノート
印刷プレビュー

反応式

HRID 1274599 の反応式
[CH3:1][N:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][C:5](=[O:12])[N:4]([C:13]2[CH:14]=[CH:15][C:16]3[S:20][N:19]=[C:18]([CH2:21][C:22](O)=[O:23])[C:17]=3[CH:25]=2)[C:3]1=[O:26].C(N1C=CN=C1)([N:29]1C=CN=C1)=O.[Cl-].[NH4+].N.Cl>O1CCCC1.CO.C(Cl)Cl>[CH3:1][N:2]1[C:7]([C:8]([F:10])([F:11])[F:9])=[CH:6][C:5](=[O:12])[N:4]([C:13]2[CH:14]=[CH:15][C:16]3[S:20][N:19]=[C:18]([CH2:21][C:22]([NH2:29])=[O:23])[C:17]=3[CH:25]=2)[C:3]1=[O:26]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 25517Ammonium ChlorideHCID 682631,1'-CarbonyldiimidazoleHCID 221199035-[3,6-Dihydro-3-methyl-2,6-dioxo-4-(trifluoromethyl)-1(2H)-pyrimidinyl]-1,2-benzisothiazole-3-acetic acid

生成物 1

HCID 22119869
5-[3,6-Dihydro-3-methyl-2,6-dioxo-4-(trifluoromethyl)-1(2H)-pyrimidinyl]-1,2-benzisothiazole-3-acetamide

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 5-[3,6-dihydro-3-methyl-2,6-dioxo-4-(trifluoromethyl)-1(2H)-pyrimidinyl]-1,2-benzisothiazole-3-acetic acid (0.960 g, 0.00250 mol) and 1,1'-carbonyldiimidazole (0.420 g, 0.00259 mol) in tetrahydrofuran is stirred at room temperature for 4.5 hours, treated with ammonium chloride (0.230 g, 0.00430 mol), stirred overnight at room temperature, treated with concentrated ammonia (1.00 mL), stirred for 5 minutes, acidified with 10% hydrochloric acid, and concentrated in vacuo to obtain a residue. The residue is diluted with a 5% methanol in methylene chloride solution and the resultant mixture is stirred for three hours and filtered to obtain a solid. The solid is washed with a 5% methanol in methylene chloride solution, slurried in water, filtered, and dried to give the title product as a white solid which is identified by NMR spectral analysis.

後処理

  1. stirringstirred overnight at room temperature
  2. stirringstirred for 5 minutes
  3. concentrationconcentrated in vacuo
  4. customto obtain a residue
  5. filtrationfiltered
  6. customto obtain a solid
  7. washThe solid is washed with a 5% methanol in methylene chloride solution
  8. filtrationfiltered
  9. customdried

出典と根拠

ORDレコード
ord-69b9d7c892074a91beeb229378589c92
出典データセット
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06156700

反応ノート

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