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tert-Butanol → HCID 66997778, 화합물

HRID 2426461
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HRID 2426461 반응식
[C:1]([O:5][C:6](=[O:34])[CH2:7][N:8]1[C:17](=[O:18])[C:16]([O:19][CH3:20])=[C:15]2[C:10]([CH2:11][CH2:12][N:13]([CH2:22][C:23]3[CH:28]=[CH:27][C:26]([F:29])=[C:25]([Cl:30])[CH:24]=3)[C:14]2=[O:21])=[C:9]1C(O)=O)([CH3:4])([CH3:3])[CH3:2].C([N:37]([CH2:40]C)CC)C.C1(P(N=[N+]=[N-])(C2C=CC=CC=2)=[O:49])C=CC=CC=1.O1CCOCC1.[C:65]([OH:69])([CH3:68])([CH3:67])[CH3:66]>>[C:65]([O:69][C:40]([NH:37][C:9]1[N:8]([CH2:7][C:6]([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:34])[C:17](=[O:18])[C:16]([O:19][CH3:20])=[C:15]2[C:10]=1[CH2:11][CH2:12][N:13]([CH2:22][C:23]1[CH:28]=[CH:27][C:26]([F:29])=[C:25]([Cl:30])[CH:24]=1)[C:14]2=[O:21])=[O:49])([CH3:68])([CH3:67])[CH3:66]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 5

HCID 6386tert-ButanolHCID 8471TriethylamineHCID 312751,4-DioxaneHCID 199401P,P-Diphenylphosphinic azideHCID 669968852-(2-tert-Butoxy-2-oxoethyl)-6-(3-chloro-4-fluorobenzyl)-4-methoxy-3,5-dioxo-2,3,5,6,7,8-hexahydro-2,6-naphthyridine-1-carboxylic acid

생성물 1

HCID 66997778
HCID 66997778, 화합물

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온도
90 °C

실험 절차

A mixture of 2-(2-tert-butoxy-2-oxoethyl)-6-(3-chloro-4-fluorobenzyl)-4-methoxy-3,5-dioxo-2,3,5,6,7,8-hexahydro-2,6-naphthyridine-1-carboxylic acid (0.31 g, 0.62 mmol), triethylamine (0.10 mL, 0.74 mmol), and diphenylphosphoryl azide (0.19 g, 0.69 mmol) in a mixture of anhydrous dioxane (6 mL) and anhydrous tert-butanol (6 mL) was heated at 90° C. overnight. The reaction mixture was concentrated under vacuum. The residue was subject to column chromatography on silica gel. Collection and concentration of appropriate fractions provided the title compound. ES MS M+1=566

후처리

  1. concentrationThe reaction mixture was concentrated under vacuum
  2. customCollection and concentration of appropriate fractions

출처 및 근거

ORD 기록
ord-db99c5780f3f45879db63ee99cdad588
출처 데이터셋
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07968564B2

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