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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Potassium Carbonate → HCID 10272690、化合物

HRID 2307734
ノート
印刷プレビュー

反応式

HRID 2307734 の反応式
[C:1]([O:4][C@H:5]1[C@@H:11]([O:12][C:13](=[O:15])[CH3:14])[C@H:10]([O:16][C:17](=[O:19])[CH3:18])[C@@H:9]([CH2:20][O:21][C:22](=[O:24])[CH3:23])[O:8][CH:6]1[OH:7])(=[O:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+].C([O:38][C:39](=[O:42])[CH2:40]Br)C1C=CC=CC=1.COC(C)(C)C>S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.O1CCOCC1>[C:1]([O:4][C@H:5]1[C@@H:11]([O:12][C:13](=[O:15])[CH3:14])[C@H:10]([O:16][C:17](=[O:19])[CH3:18])[C@@H:9]([CH2:20][O:21][C:22](=[O:24])[CH3:23])[O:8][CH:6]1[O:7][CH2:40][C:39]([OH:42])=[O:38])(=[O:3])[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 11430Potassium CarbonateHCID 15413tert-Butyl methyl etherHCID 62576Benzyl bromoacetateHCID 117598232,3,4,6-TETRA-O-ACETYL-D-MANNOPYRANOSE

生成物 1

HCID 10272690HCID 10272690、化合物

試薬・触媒・溶媒 2

HCID 94433
Tetrabutylammonium hydrogen sulfate
触媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
0 °C

実験手順

A mixture that consists of 34.83 g (100 mmol) of 2,3,4,6-tetra-O-acetyl-mannopyranose, 1.70 g (5 mmol) of tetrabutylammonium hydrogen sulfate and 82.93 g (600 mmol) of fine-powder potassium carbonate in 350 ml of dioxane is cooled to 0° C. At 0° C., 34.36 g (150 mmol) of bromoacetic acid benzyl ester is added in drops over 10 minutes while being stirred vigorously. It is stirred for one hour at 0° C. 250 ml of MTB (methyl-tert-butyl ether) is added, solid is filtered out, and the filtrate is evaporated to the dry state in a vacuum. The residue is taken up in 500 ml of ethanol. 5 g of palladium (10%) on activated carbon is added thereto and hydrogenated until no more hydrogen is taken up by the solution. Catalyst is filtered out, it is rewashed with ethanol, and the combined solutions are evaporated to the dry state in a vacuum.

後処理

  1. stirringIt is stirred for one hour at 0° C
  2. filtrationsolid is filtered out
  3. customthe filtrate is evaporated to the dry state in a vacuum
  4. addition5 g of palladium (10%) on activated carbon is added
  5. filtrationCatalyst is filtered out
  6. customthe combined solutions are evaporated to the dry state in a vacuum

出典と根拠

ORDレコード
ord-a4e7ed4d94624b7cb647fe21af629e3d
出典データセット
uspto-grants-2004_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06831164B2

反応ノート

読み込み中…

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