Hydrochloric Acid → 9-Iodo-3,4,7,8-tetrahydro-[1,4]diazepino[7,1-a]isoquinoline-2,5-dione

HRID 532874노트

반응식

HRID 532874 반응식
[Cl-].[C:2]([CH2:5][CH:6]1[C:15]2[C:10](=[C:11]([I:16])[CH:12]=[CH:13][CH:14]=2)[CH2:9][CH2:8][N:7]1[C:17](=[O:20])[CH2:18][NH3+:19])(O)=[O:3].C(OC(NCC(N1CCC2C(=CC=CC=2I)C1CC([O-])=O)=O)=O)(C)(C)C.[Na+].Cl>O1CCOCC1>[I:16][C:11]1[CH:12]=[CH:13][CH:14]=[C:15]2[C:10]=1[CH2:9][CH2:8][N:7]1[C:17](=[O:20])[CH2:18][NH:19][C:2](=[O:3])[CH:5]=[C:6]12

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 86711322Sodium 2-(2-(2-((tert-butoxycarbonyl)amino)acetyl)-5-iodo-1,2,3,4-tetrahydroisoquinolin-1-yl)acetateHCID 867113252-(1-(carboxymethyl)-5-iodo-3,4-dihydroisoquinolin-2(1H)-yl)-2-oxoethanaminium chloride

생성물 1

HCID 867113799-Iodo-3,4,7,8-tetrahydro-[1,4]diazepino[7,1-a]isoquinoline-2,5-dione

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

2-(1-(carboxymethyl)-5-iodo-3,4-dihydroisoquinolin-2(1H)-yl)-2-oxoethanaminium chloride. A suspension of sodium 2-(2-(2-((tert-butoxycarbonyl)amino)acetyl)-5-iodo-1,2,3,4-tetrahydroisoquinolin-1-yl)acetate (49.8 g, 100 mmol) in dry dioxane (1 L) was treated with an aqueous solution of HCl (4M, 280 ml, 1.12 mol) and the mixture was stirred at RT for 18 h. The reaction mixture was then concentrated in vacuo to give the title compound (46.1 g) as a beige powder that was used as it is in the next step. UPLC-MS: MS 375.1 (M+H+); UPLC rt 0.60 min.

후처리

  1. concentrationThe reaction mixture was then concentrated in vacuo

출처 및 근거

ORD 기록
ord-51cb428dae54415a92b4352b7dfe8c1e
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08853203B2

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