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Formaldehyde → 3-(3-Dimethylcarbamoyl-4-methoxy-5-trifluoromethylbenzoyl)-2,3-dihydro-1,3-benzothiazole

HRID 385111
ノート
印刷プレビュー

反応式

HRID 385111 の反応式
[S:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[NH:3][CH2:2]1.NC1C=CC=CC=1S.C=O.[CH3:20][N:21]([CH3:39])[C:22]([C:24]1[CH:25]=[C:26]([CH:30]=[C:31]([C:35]([F:38])([F:37])[F:36])[C:32]=1[O:33][CH3:34])[C:27](Cl)=[O:28])=[O:23]>C(Cl)(Cl)Cl.C(N(CC)CC)C>[CH3:39][N:21]([CH3:20])[C:22]([C:24]1[CH:25]=[C:26]([CH:30]=[C:31]([C:35]([F:36])([F:38])[F:37])[C:32]=1[O:33][CH3:34])[C:27]([N:3]1[C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=2[S:1][CH2:2]1)=[O:28])=[O:23]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 712FormaldehydeHCID 87132-AminothiophenolHCID 96588BenzothiazolineHCID 866681743-Dimethylcarbamoyl-4-methoxy-5-trifluoromethylbenzoyl chloride

生成物 1

HCID 681087933-(3-Dimethylcarbamoyl-4-methoxy-5-trifluoromethylbenzoyl)-2,3-dihydro-1,3-benzothiazole

試薬・触媒・溶媒 2

HCID 6212
Chloroform
溶媒
HCID 8471Triethylamine溶媒

実験手順

2,3-dihydro-1,3-benzothiazole synthesized from 2-aminobenzenethiol (214 mg) and 37% formalin (0.14 mL) in the same manner as in Example 1 was dissolved in chloroform (4 mL), and triethylamine (0.47 mL) and 3-dimethylcarbamoyl-4-methoxy-5-trifluoromethylbenzoyl chloride were added to the solution, and then the mixture was stirred at room temperature for 1 hour. The solvent was distilled off under reduced pressure and water was added, and then the mixture was extracted with ethyl acetate. The organic layer was washed with 1N hydrochloric acid, 1N sodium hydroxide and saturated brine, and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure and the obtained residue was used for the synthesis of (g).

後処理

  1. distillationThe solvent was distilled off under reduced pressure and water
  2. additionwas added
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with 1N hydrochloric acid, 1N sodium hydroxide and saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationThe solvent was distilled off under reduced pressure
  7. customthe obtained residue was used for the synthesis of (g)

出典と根拠

ORDレコード
ord-23f7dd08c3ae49518d72d25143e9b4e8
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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