ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
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
  1. ホーム
  2. /反応

Sulfuric Acid → UV-328

HRID 257652
ノート
印刷プレビュー

反応式

HRID 257652 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[N:10]=[N:11][C:12]1[CH:17]=[C:16]([C:18]([CH2:21][CH3:22])([CH3:20])[CH3:19])[CH:15]=[C:14]([C:23]([CH2:26][CH3:27])([CH3:25])[CH3:24])[C:13]=1[OH:28])([O-])=O.[OH-].[Na+].C1C2C(=O)C3C(=CC=CC=3)C=2C=CC=1.O=C[C@@H]([C@H]([C@@H]([C@@H](CO)O)O)O)O.S(=O)(=O)(O)O>O.CO>[OH:28][C:13]1[C:14]([C:23]([CH2:26][CH3:27])([CH3:25])[CH3:24])=[CH:15][C:16]([C:18]([CH2:21][CH3:22])([CH3:20])[CH3:19])=[CH:17][C:12]=1[N:11]1[N:10]=[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]2=[N:1]1
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

8

反応物 5

HCID 1118Sulfuric AcidHCID 10241FluorenoneHCID 14798Sodium HydroxideHCID 1041112-Nitro-2'-hydroxy-3',5'-bis(tert-amyl)azobenzeneHCID 107526(2R,3S,4R,5R)-2,3,4,5,6-pentahydroxyhexanal

生成物 1

HCID 33263UV-328収率 85%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒2 回

反応条件

温度
20 °C

実験手順

Example 1 from U.S. Pat. No. 4,835,284 is duplicated. 2-nitro-2'-hydroxy-3',5'-di-t-amylazobenzene (12.8 g) is added to a mixture of methanol (41 g), water (10 g) and 97% sodium hydroxide (11 g), and the resultant mixture is stirred at 65° C. for 30 minutes. Thereafter, 9-fluorenone (2.0 g) and then glucose (12 g) are added to the mixture at 60° C. to 65° C. over 4 hours. The resultant mixture is further stirred for 4 hours at the boiling point (70° C.), thus completing the reduction reaction. Thereafter, water (50 ml) is added to the reaction liquor, and the reaction liquor is neutralized with 62% sulfuric acid (13 g). The liquor thus neutralized is cooled to 20° C. to precipitate a crystal. The crystal thus obtained is separated by filtration, and the separated crystal is fully washed with water and further with methanol. The washed crystal is then dried, thus producing 9.9 g of 2-(2'-hydroxy-3',5'-di-t-amylphenyl)-benzotriazole having a melting point of 77° to 79° C. at the yield of 85.0%. One can see that reduction using the aromatic ketone 9-fluorenone takes over 81/2 hours.

後処理

  1. customthe reduction reaction
  2. customto precipitate a crystal
  3. customThe crystal thus obtained
  4. customis separated by filtration
  5. washthe separated crystal is fully washed with water and further with methanol
  6. customThe washed crystal is then dried

出典と根拠

ORDレコード
ord-5f49b659648e41138f6f7932b8dde1fd
出典データセット
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05262541

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート