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Hydrochloric Acid → HCID 68108353、化合物

HRID 385028
ノート
印刷プレビュー

反応式

HRID 385028 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:16]=[C:17]([C:21]#[N:22])[C:18]=1[O:19]C)[C:5]([N:7]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[S:9][CH2:8]1)=[O:6].[Cl-].[Li+].Cl>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[C:4]([CH:16]=[C:17]([C:21]#[N:22])[C:18]=1[OH:19])[C:5]([N:7]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[S:9][CH2:8]1)=[O:6]
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 313Hydrochloric AcidHCID 433294Lithium ChlorideHCID 681080913-(3-Chloro-5-cyano-4-methoxybenzoyl)-2,3-dihydro-1,3-benzothiazole

生成物 1

HCID 68108353HCID 68108353、化合物収率 33.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

3-(3-chloro-5-cyano-4-methoxybenzoyl)-2,3-dihydro-1,3-benzothiazole (213 mg) was dissolved in N,N-dimethylformamide (2 mL), and lithium chloride (111 mg) was added to the solution, and then the mixture was stiffed at 100° C. for 2 hours. To the reaction solution, 1N hydrochloric acid was added, and then the reaction mixture was extracted with ethyl acetate. The organic layer was washed with 1N hydrochloric acid and saturated brine, and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure and the obtained residue was purified by silica gel column chromatography (ethyl acetate:methanol=10:1), and then crystallized from n-hexane-chloroform to obtain the title compound (68 mg) as a pale yellow crystal.

後処理

  1. extractionthe reaction mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with 1N hydrochloric acid and saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationThe solvent was distilled off under reduced pressure
  5. customthe obtained residue was purified by silica gel column chromatography (ethyl acetate:methanol=10:1)
  6. customcrystallized from n-hexane-chloroform

出典と根拠

ORDレコード
ord-0e563d028bec44f8ba754077fcaa184e
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08367843B2

反応ノート

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