Boron trifluoride etherate → Bis-(8-methoxycarbonyl-2,2,6,6-tetramethylbenzo[1,2-d:4,5-d']-bis(1,3)dioxol-4-yl)-mono-(8-methoxycarbonyl-2,2,6,6-tetramethylbenzo[1,2-d:4,5-d']-bis(1,3)dithiol-4-yl)methane

HRID 1108173

反応式

HRID 1108173 の反応式
[CH3:1][O:2][C:3]([C:5]1[C:16]2[O:15][C:14]([CH3:18])([CH3:17])[O:13][C:12]=2[C:11]([C:19]([C:41]2[C:51]3[O:52][C:53]([CH3:56])([CH3:55])[O:54][C:50]=3[C:49]([C:57]([O:59][CH3:60])=[O:58])=[C:43]3[O:44][C:45]([CH3:48])([CH3:47])[O:46][C:42]=23)([C:21]2[C:31]3[S:32][C:33]([CH3:36])([CH3:35])[S:34][C:30]=3[C:29]([C:37]([O:39][CH3:40])=[O:38])=[C:23]3[S:24][C:25]([CH3:28])([CH3:27])[S:26][C:22]=23)O)=[C:10]2[C:6]=1[O:7][C:8]([CH3:62])([CH3:61])[O:9]2)=[O:4].B(F)(F)F.CCOCC.[Sn](Cl)Cl>[Zn]>[CH3:60][O:59][C:57]([C:49]1[C:50]2[O:54][C:53]([CH3:55])([CH3:56])[O:52][C:51]=2[C:41]([CH:19]([C:11]2[C:12]3[O:13][C:14]([CH3:18])([CH3:17])[O:15][C:16]=3[C:5]([C:3]([O:2][CH3:1])=[O:4])=[C:6]3[O:7][C:8]([CH3:61])([CH3:62])[O:9][C:10]=23)[C:21]2[C:31]3[S:32][C:33]([CH3:36])([CH3:35])[S:34][C:30]=3[C:29]([C:37]([O:39][CH3:40])=[O:38])=[C:23]3[S:24][C:25]([CH3:27])([CH3:28])[S:26][C:22]=23)=[C:42]2[C:43]=1[O:44][C:45]([CH3:48])([CH3:47])[O:46]2)=[O:58]

参加物

5

反応物 3

HCID 8000Boron trifluoride etherateHCID 24479Stannous ChlorideHCID 86752299Bis-(8-methoxycarbonyl-2,2,6,6-tetramethylbenzo[1,2-d:4,5-d']-bis(1,3)dioxol-4-yl)-mono-(8-methoxycarbonyl-2,2,6,6-tetramethylbenzo[1,2-d:4,5-d']-bis(1,3)dithiol-4-yl)methanol

生成物 1

HCID 86752298Bis-(8-methoxycarbonyl-2,2,6,6-tetramethylbenzo[1,2-d:4,5-d']-bis(1,3)dioxol-4-yl)-mono-(8-methoxycarbonyl-2,2,6,6-tetramethylbenzo[1,2-d:4,5-d']-bis(1,3)dithiol-4-yl)methane

試薬・触媒・溶媒 1

HCID 23994Zinc触媒

実験手順

Bis-(8-methoxycarbonyl-2,2,6,6-tetramethylbenzo[1,2-d:4,5-d']-bis(1,3)dioxol-4-yl)-mono-(8-methoxycarbonyl-2,2,6,6-tetramethylbenzo[1,2-d:4,5-d']-bis(1,3)dithiol-4-yl)methanol (5 mg, 0.005 mmol) was dissolved in dry, degassed acetonitrile under an argon atmosphere. BF3.Et2O (2.0 μL, 0.011 mmol) and tin(II) chloride (3.0 mg, 0.016 mmol) were added. Amalgamated zinc (1.0 mg, 0.015 mmol), was added. The product was purified by flash chromatography (ether/heptane 5:1). Due to the small amount used the yield was not determined.

後処理

  1. customin dry
  2. customdegassed acetonitrile under an argon atmosphere
  3. customThe product was purified by flash chromatography (ether/heptane 5:1)

出典と根拠

ORDレコード
ord-92d507764bac4f08816881f205c8fc7c
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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