Carbon Dioxide → Bis-(8-carboxy-2,2,6,6-tetramethylbenzo[1,2-d:4,5-d']-bis(1,3)-dioxol-4-yl)-mono-(8-carboxy-2,2,6,6-tetramethylbenzo[1,2-d:4,5-d']-bis(1,3)dithiol-4-yl)methanol

참여 물질

역할	이름	HCID	투입량
반응물	Carbon Dioxide	HCID 280	—
반응물	N,N,N',N'-Tetramethylethylenediamine	HCID 8037	—
반응물	Bis-(2,2,6,6-tetramethylbenzo[1,2-d:4,5-d']-bis(1,3)dioxol-4-yl)-mono-(2,2,6,6-tetramethylbenzo[1,2-d:4,5-d']-bis(1,3)dithiole-4-yl)methanol	HCID 86752296	—
반응물	HCID 178418306	HCID 178418306	—
용매	Diethyl Ether	HCID 3283	—
용매	Cyclohexane	HCID 8078	—
생성물	Bis-(8-carboxy-2,2,6,6-tetramethylbenzo[1,2-d:4,5-d']-bis(1,3)-dioxol-4-yl)-mono-(8-carboxy-2,2,6,6-tetramethylbenzo[1,2-d:4,5-d']-bis(1,3)dithiol-4-yl)methanol	HCID 86752297	—

반응 단계

Dry TMEDA (1.21 mL, 8.04 mmol) and t-butyllithium (5.36 mL, 1.5M in pentane) were dissolved in dry cyclohexane (12 mL) at 0° C. Bis-(2,2,6,6-tetramethylbenzo[1,2-d:4,5-d']-bis(1,3)dioxol-4-yl)-mono-(2,2,6,6-tetramethylbenzo[1,2-d:4,5-d']-bis(1,3)dithiol-4-yl)methanol (0.608 g, 0.804 mmol) was then added at ambient temperature as a solid. After 20 min, solid carbon dioxide was added followed by dry ether (50 mL). After stirring for 17 h, the reaction mixture was filtered and the precipitate was dried. The acid was purified by preparative HPLC. Yield 0.285 g (40%).

출처 및 근거

DOI	10.6084/m9.figshare.5104873.v1
특허 번호	US06063360
출처 데이터셋	uspto-grants-2000_05
ORD ID	ord-56a0c6a20bb74d3dbca1250523b58c39
출처 메모	uspto-grants-2000_05