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Ammonium Chloride → 2-(6-(4-chlorophenyl)-1-methyl-5,6-dihydro-4H-benzo[b][1,2,4]triazolo[4,3-d][1,4]diazepin-4-yl) ethanol

HRID 1485403
ノート
印刷プレビュー

反応式

HRID 1485403 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:14](=O)[CH:13]([CH2:16][C:17](O)=[O:18])[C:12]3=[N:20][N:21]=[C:22]([CH3:23])[N:11]3[C:10]3[CH:24]=[CH:25][CH:26]=[CH:27][C:9]2=3)=[CH:4][CH:3]=1.[NH4+].[Cl-]>C1COCC1>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:14][CH:13]([CH2:16][CH2:17][OH:18])[C:12]3=[N:20][N:21]=[C:22]([CH3:23])[N:11]3[C:10]3[CH:24]=[CH:25][CH:26]=[CH:27][C:9]2=3)=[CH:4][CH:3]=1
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 25517Ammonium ChlorideHCID 709789952-(6-(4-chlorophenyl)-1-methyl-5-oxo-5,6-dihydro-4H-benzo[b][1,2,4]triazolo[4,3-d][1,4]diazepin-4-yl)acetic acid

生成物 1

HCID 709790752-(6-(4-chlorophenyl)-1-methyl-5,6-dihydro-4H-benzo[b][1,2,4]triazolo[4,3-d][1,4]diazepin-4-yl) ethanol収率 19.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of 2-(6-(4-chlorophenyl)-1-methyl-5-oxo-5,6-dihydro-4H-benzo[b][1,2,4]triazolo[4,3-d][1,4]diazepin-4-yl)acetic acid (500 mg, 1.32 mmol) in THF (300 ml) was added BH3 solution in THF (1 M, 6.5 mL) dropwise, the resulting mixture was stirred at room temperature overnight. NH4Cl aqueous (15 mL) was added, and then extracted with DCM (3×30 mL), the combined organic layers were dried over Na2SO4, and the solvent was removed in vacuum. The residue was purified by flash chromatography eluting with DCM:MeOH=40:1 to give 2-(6-(4-chlorophenyl)-1-methyl-5,6-dihydro-4H-benzo[b][1,2,4]triazolo[4,3-d][1,4]diazepin-4-yl)ethanol as an off-white solid (90 mg, 18.5%).

後処理

  1. extractionextracted with DCM (3×30 mL)
  2. dry with materialthe combined organic layers were dried over Na2SO4
  3. customthe solvent was removed in vacuum
  4. customThe residue was purified by flash chromatography
  5. washeluting with DCM

出典と根拠

ORDレコード
ord-b2624bbf5f9a4dde9db3f65370837b52
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09422292B2

反応ノート

読み込み中…

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