Trimethyl orthoformate → HCID 136060816, 화합물

HRID 1851433노트

반응식

[NH:1]([C:3]([C:5]1[NH:6][C:7]2[C:12]([CH:13]=1)=[CH:11][CH:10]=[CH:9][C:8]=2[NH:14][S:15]([C:18]1[S:19][CH:20]=[CH:21][CH:22]=1)(=[O:17])=[O:16])=[O:4])[NH2:2].[CH:23](OC)(OC)OC>>[O:4]1[CH:23]=[N:2][N:1]=[C:3]1[C:5]1[NH:6][C:7]2[C:12]([CH:13]=1)=[CH:11][CH:10]=[CH:9][C:8]=2[NH:14][S:15]([C:18]1[S:19][CH:20]=[CH:21][CH:22]=1)(=[O:17])=[O:16]

참가 물질

반응물 2

HCID 9005Trimethyl orthoformate

HCID 57901816HCID 57901816, 화합물

생성물 1

HCID 136060816HCID 136060816, 화합물수율 39%

반응 조건

온도: 100 °C

실험 절차

A mixture of N-[2-(hydrazinocarbonyl)-1H-indol-7-yl]thiophene-2-sulfonamide (0.28 g) and trimethyl orthoformate (0.13 g) was stirred at 100° C. overnight. The reaction mixture was concentrated, and the residue was subjected to silica gel column chromatography and the title compound (0.11 g, yield 39%) was obtained as colorless crystals from a fraction eluted with tetrahydrofuran-hexane (1:1, volume ratio). The crystals were recrystallized from ethyl acetate-hexane. melting point 271-272° C. (decomposition).

후처리

concentrationThe reaction mixture was concentrated

출처 및 근거

ORD 기록: ord-ceb5f298409c445dad463bbc1eeeb38c
출처 데이터셋: uspto-grants-2015_02
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08957070B2

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