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

HRID 1108172

反応式

HRID 1108172 の反応式
CN(CCN(C)C)C.C([Li])(C)(C)C.[CH3:14][C:15]1([CH3:63])[O:19][C:18]2[C:20]([C:29]([C:47]3[C:57]4[O:58][C:59]([CH3:62])([CH3:61])[O:60][C:56]=4[CH:55]=[C:49]4[O:50][C:51]([CH3:54])([CH3:53])[O:52][C:48]=34)([C:31]3[C:41]4[S:42][C:43]([CH3:46])([CH3:45])[S:44][C:40]=4[CH:39]=[C:33]4[S:34][C:35]([CH3:38])([CH3:37])[S:36][C:32]=34)[OH:30])=[C:21]3[O:25][C:24]([CH3:27])([CH3:26])[O:23][C:22]3=[CH:28][C:17]=2[O:16]1.[C:64](=[O:66])=[O:65]>C1CCCCC1.CCOCC>[C:64]([C:28]1[C:22]2[O:23][C:24]([CH3:26])([CH3:27])[O:25][C:21]=2[C:20]([C:29]([C:47]2[C:48]3[O:52][C:51]([CH3:54])([CH3:53])[O:50][C:49]=3[C:55]([C:24]([OH:25])=[O:23])=[C:56]3[O:60][C:59]([CH3:62])([CH3:61])[O:58][C:57]=23)([C:31]2[C:32]3[S:36][C:35]([CH3:37])([CH3:38])[S:34][C:33]=3[C:39]([C:15]([OH:19])=[O:16])=[C:40]3[S:44][C:43]([CH3:45])([CH3:46])[S:42][C:41]=23)[OH:30])=[C:18]2[C:17]=1[O:16][C:15]([CH3:63])([CH3:14])[O:19]2)([OH:66])=[O:65]

参加物

7

反応物 4

HCID 280Carbon DioxideHCID 8037N,N,N',N'-TetramethylethylenediamineHCID 86752296Bis-(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)methanolHCID 178418306HCID 178418306、化合物

生成物 1

HCID 86752297Bis-(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

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8078Cyclohexane溶媒

実験手順

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%).

後処理

  1. filtrationthe reaction mixture was filtered
  2. customthe precipitate was dried
  3. customThe acid was purified by preparative HPLC

出典と根拠

ORDレコード
ord-56a0c6a20bb74d3dbca1250523b58c39
出典データセット
uspto-grants-2000_05
特許番号
US06063360

関連ノート

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