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Hydrochloric Acid → HCID 178493965、化合物

HRID 1864633
ノート
印刷プレビュー

反応式

HRID 1864633 の反応式
[Li+].[OH-].[O:3]=[C:4]1[N:10]([CH:11]2[CH2:16][CH2:15][N:14]([C:17]([O:19][C@@H:20]([C:34]([O:36]C)=[O:35])[CH2:21][C:22]3[CH:32]=[C:31]([CH3:33])[C:25]4[NH:26][C:27]([O:29][CH3:30])=[N:28][C:24]=4[CH:23]=3)=[O:18])[CH2:13][CH2:12]2)[CH2:9][CH2:8][C:7]2[CH:38]=[CH:39][CH:40]=[CH:41][C:6]=2[NH:5]1.Cl>O.C1COCC1>[O:3]=[C:4]1[N:10]([CH:11]2[CH2:12][CH2:13][N:14]([C:17]([O:19][C@@H:20]([C:34]([OH:36])=[O:35])[CH2:21][C:22]3[CH:32]=[C:31]([CH3:33])[C:25]4[NH:26][C:27]([O:29][CH3:30])=[N:28][C:24]=4[CH:23]=3)=[O:18])[CH2:15][CH2:16]2)[CH2:9][CH2:8][C:7]2[CH:38]=[CH:39][CH:40]=[CH:41][C:6]=2[NH:5]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 178501366HCID 178501366、化合物

生成物 1

HCID 178493965HCID 178493965、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 0.10 g (4.18 mmol) LiOH in 6 mL water was added to a solution of 0.98 g (1.83 mmol) (R)-1-methoxycarbonyl-2-(2-methoxy-7-methyl-1H-benzimidazol-5-yl)-ethyl 4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidine-1-carboxylate in 18 mL THF and the reaction solution was stirred overnight at RT. 1.05 mL of 4 M HCl was added and the THF was eliminated i.vac. The mixture was decanted to separate off the oily residue, this was dissolved in DCM/MeOH and the organic phase was dried on Na2SO4. After the desiccant and solvent had been eliminated the desired product was obtained.

後処理

  1. customThe mixture was decanted
  2. customto separate off the oily residue
  3. dissolutionthis was dissolved in DCM/MeOH
  4. customthe organic phase was dried on Na2SO4
  5. customwas obtained

出典と根拠

ORDレコード
ord-013b256e28a441b7b470bbb29bd585b1
出典データセット
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07625886B2

反応ノート

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