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

Ethyl Acetate → HCID 10279786、化合物

HRID 2396260
ノート
印刷プレビュー

反応式

HRID 2396260 の反応式
[CH:1]([C:4]1[CH:11]=[C:10]([CH:12]([CH3:14])[CH3:13])[CH:9]=[C:8]([CH:15]([CH3:17])[CH3:16])[C:5]=1[CH2:6]Br)([CH3:3])[CH3:2].[CH:18]([C:21]1[CH:33]=[CH:32][CH:31]=[C:30]([CH:34]([CH3:36])[CH3:35])[C:22]=1[O:23][S:24]([N:27]=C=O)(=[O:26])=[O:25])([CH3:20])[CH3:19].[NH4+].[Cl-].C[CH2:40][O:41]C(C)=O>C1COCC1>[CH3:2][CH:1]([C:4]1[CH:11]=[C:10]([CH:12]([CH3:14])[CH3:13])[CH:9]=[C:8]([CH:15]([CH3:17])[CH3:16])[C:5]=1[CH2:6][C:40]([C:33]1[C:21]([CH:18]([CH3:19])[CH3:20])=[C:22]([O:23][S:24](=[O:25])(=[O:26])[NH2:27])[C:30]([CH:34]([CH3:35])[CH3:36])=[CH:31][CH:32]=1)=[O:41])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8857Ethyl AcetateHCID 25517Ammonium ChlorideHCID 10590086HCID 10590086、化合物HCID 106367162,6-Diisopropylphenoxysulfonyl isocyanate

生成物 1

HCID 10279786HCID 10279786、化合物収率 67%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran
溶媒
2 回

実験手順

A solution of 2,4,6 - triisopropylbenzyl bromide (12 g, 40.4 mmol) in dry THF (160 mL) was added to a suspension of Mg powder (1.96 g, 80.8 mmol) (4hours) in THF (20 mL) heated under reflux. 2,6-Diisopropylphenoxysulfonyl isocyanate (ROSO2NCO) (see Phos. and Sulf., 19:167 (1984) for preparation) (11.45 g, 40.4 mmol) was added neat, and after the addition was completed, the reflux was continued for another 2 hours. The reaction was stirred at room temperature for 16 hours. Saturated NH4Cl and EtOAc were added. The EtOAc layer was separated, dried over MgSO4, filtered, and evaporated to dryness. After purification by column chromatography (4:1 hexane:EtOAc), the compound was isolated as white solid (13.5 g, 67%), mp 178°-180° C.

後処理

  1. temperatureheated
  2. temperatureunder reflux
  3. additionafter the addition
  4. customThe EtOAc layer was separated
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. customevaporated to dryness
  8. customAfter purification by column chromatography (4:1 hexane:EtOAc)

出典と根拠

ORDレコード
ord-898a7081a5bf4069ba210bb5a2d32642
出典データセット
uspto-grants-1996_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05491172

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート