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1,4-Dioxane hydrochloride → 4-{2-[2-(Acetylamino)-1,3-thiazol-4-yl]ethyl}benzyl hydrazinecarboxylate hydrochloride

HRID 1892473
ノート
印刷プレビュー

反応式

HRID 1892473 の反応式
[NH:1]([C:10]([O:12][CH2:13][C:14]1[CH:19]=[CH:18][C:17]([CH2:20][CH2:21][C:22]2[N:23]=[C:24]([NH:27][C:28](=[O:30])[CH3:29])[S:25][CH:26]=2)=[CH:16][CH:15]=1)=[O:11])[NH:2]C(OC(C)(C)C)=O.O1CCOCC1.[ClH:37]>ClCCl>[ClH:37].[NH:1]([C:10]([O:12][CH2:13][C:14]1[CH:15]=[CH:16][C:17]([CH2:20][CH2:21][C:22]2[N:23]=[C:24]([NH:27][C:28](=[O:30])[CH3:29])[S:25][CH:26]=2)=[CH:18][CH:19]=1)=[O:11])[NH2:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 204431481,4-Dioxane hydrochlorideHCID 86649981HCID 86649981、化合物

生成物 1

HCID 866499824-{2-[2-(Acetylamino)-1,3-thiazol-4-yl]ethyl}benzyl hydrazinecarboxylate hydrochloride収率 103.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a suspension of 4-{2-[2-(acetylamino)-1,3-thiazol-4-yl]ethyl}benzyl tert-butyl hydrazine-1,2-dicarboxylate (203.0 mg, 0.467 mmol) in anhydrous dichloromethane (2.3 ml) was added 4M hydrogen chloride dioxane solution (2.3 ml, 9.2 mmol). After stirring at room temperature for 2.5 hr, the mixture was concentrated under reduced pressure. Ethyl acetate was added to the concentrated residue, and the mixture was concentrated again under reduced pressure. This operation was performed 3 times to remove hydrogen chloride gas azeotropically. The residue was suspended in ethyl acetate and filtered. The filtered product was washed with ethyl acetate and dried under reduced pressure to give the title compound (179.3 mg, quantitative) as a white solid.

後処理

  1. concentrationthe mixture was concentrated under reduced pressure
  2. additionEthyl acetate was added to the concentrated residue
  3. concentrationthe mixture was concentrated again under reduced pressure
  4. customto remove hydrogen chloride gas azeotropically
  5. filtrationfiltered
  6. washThe filtered product was washed with ethyl acetate
  7. customdried under reduced pressure

出典と根拠

ORDレコード
ord-eeb3a8e140124b1f95614280c4b07c9b
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08507690B2

反応ノート

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