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Hydrochloric Acid → HCID 178493965, 화합물

HRID 1864633
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HRID 1864633 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 178501366HCID 178501366, 화합물

생성물 1

HCID 178493965HCID 178493965, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-013b256e28a441b7b470bbb29bd585b1
출처 데이터셋
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07625886B2

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