Hydrochloric Acid → N-[5-(2,3,4,5-tetrahydro-1,4-benzoxazepin-7-yl)-1,3-thiazol-2-yl]acetamide hydrochloride

HRID 473852ノート

反応式

HRID 473852 の反応式
[C:1]([NH:4][C:5]1[S:6][C:7]([C:10]2[CH:11]=[CH:12][C:13]3[O:19][CH2:18][CH2:17][N:16](C(OC(C)(C)C)=O)[CH2:15][C:14]=3[CH:27]=2)=[CH:8][N:9]=1)(=[O:3])[CH3:2].[ClH:28]>CO.O1CCOCC1>[ClH:28].[O:19]1[C:13]2[CH:12]=[CH:11][C:10]([C:7]3[S:6][C:5]([NH:4][C:1](=[O:3])[CH3:2])=[N:9][CH:8]=3)=[CH:27][C:14]=2[CH2:15][NH:16][CH2:17][CH2:18]1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 59604271tert-butyl 7-[2-(acetylamino)-1,3-thiazol-5-yl]-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate

生成物 1

HCID 86647837N-[5-(2,3,4,5-tetrahydro-1,4-benzoxazepin-7-yl)-1,3-thiazol-2-yl]acetamide hydrochloride収率 99%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 312751,4-Dioxane溶媒

実験手順

A mixture 1,1-dimethylethyl 7-[2-(acetylamino)-1,3-thiazol-5-yl]-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate (0.29 g, 0.75 mmol), in methanol (2 mL) and 4 M hydrogen chloride in 1,4-dioxane (2 mL) was stirred at 70° C. for 15 minutes. The reaction mixture was cooled and concentrated, and dried in vacuum to give the de-protected product N-[5-(2,3,4,5-tetrahydro-1,4-benzoxazepin-7-yl)-1,3-thiazol-2-yl]acetamide hydrochloride (0.24 g, 0.24 mmol, 99% yield); MS (EI) for C14H15N3O2S: 290 (MH+).

後処理

  1. temperatureThe reaction mixture was cooled
  2. concentrationconcentrated
  3. customdried in vacuum

出典と根拠

ORDレコード
ord-18d8360b216347a192c429957ea71773
出典データセット
uspto-grants-2014_01
特許番号
US08637499B2

反応ノート

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