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Sodium sulfate decahydrate → HCID 55026015、化合物

HRID 2422240
ノート
印刷プレビュー

反応式

HRID 2422240 の反応式
[N:1]1[C:5]2[C:6]3[C:11]([CH2:12][CH2:13][C:4]=2[S:3][C:2]=1[NH:14][C:15](=O)[CH2:16][CH3:17])=[CH:10][CH:9]=[CH:8][CH:7]=3.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.[O-]S([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[CH2:15]([NH:14][C:2]1[S:3][C:4]2[CH2:13][CH2:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[N:1]=1)[CH2:16][CH3:17]
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 62649Sodium sulfate decahydrateHCID 861848HCID 861848、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 55026015HCID 55026015、化合物収率 82%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Under ice-cooling, to a solution of N-(4,5-dihydronaphtho[1,2-d][1,3]thiazol-2-yl)propanamide (1.70 g, 6.6 mmol) in tetrahydrofuran (30 mL) was added lithium aluminum hydride (749 mg, 20 mmol), and the mixture was stirred at room temperature for 3 hrs. Sodium sulfate 10 hydrate (9.6 g, 30 mmol) was added, and the mixture was stirred at room temperature for 1 hr. Insoluble material was filtered off, and the filtrate was concentrated. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=4:1) to give the title compound (1.32 g, yield 82%) as a yellow powder.

後処理

  1. stirringthe mixture was stirred at room temperature for 1 hr
  2. filtrationInsoluble material was filtered off
  3. concentrationthe filtrate was concentrated
  4. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=4:1)

出典と根拠

ORDレコード
ord-1d49a952f8dd438abde976df9ff9f3ea
出典データセット
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07960369B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート