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

Ethanol → 4-(Docosyloxy)-alpha-[4-(docosyloxy)phenyl]benzenemethanamine

HRID 1025057
ノート
印刷プレビュー

反応式

HRID 1025057 の反応式
[CH2:1]([O:23][C:24]1[CH:29]=[CH:28][C:27]([CH:30]([NH:60]C(=O)OCC)[C:31]2[CH:36]=[CH:35][C:34]([O:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][CH2:47][CH2:48][CH2:49][CH2:50][CH2:51][CH2:52][CH2:53][CH2:54][CH2:55][CH2:56][CH2:57][CH2:58][CH3:59])=[CH:33][CH:32]=2)=[CH:26][CH:25]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH3:22].C1(C)C=CC=CC=1.C(O)C.[OH-].[Na+]>C(OCC)(=O)C.CCCCCC.O>[CH2:1]([O:23][C:24]1[CH:25]=[CH:26][C:27]([CH:30]([NH2:60])[C:31]2[CH:36]=[CH:35][C:34]([O:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][CH2:47][CH2:48][CH2:49][CH2:50][CH2:51][CH2:52][CH2:53][CH2:54][CH2:55][CH2:56][CH2:57][CH2:58][CH3:59])=[CH:33][CH:32]=2)=[CH:28][CH:29]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH3:22]
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 4

HCID 702EthanolHCID 1140TolueneHCID 14798Sodium Hydroxide2 回HCID 86646200Ethyl di(4-docosoxyphenyl)methylcarbamate

生成物 1

HCID 665753054-(Docosyloxy)-alpha-[4-(docosyloxy)phenyl]benzenemethanamine収率 98%

試薬・触媒・溶媒 3

HCID 962
Water
溶媒
HCID 8058Hexane溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
100 °C

実験手順

To crude crystals (31.9 g) of ethyl di(4-docosoxyphenyl)methylcarbamate were added toluene (300 mL), ethanol (200 mL), and sodium hydroxide (4.2 g, 105 mmol), and the mixture was refluxed under stirring at 100° C. Sodium hydroxide (total 9.8 g, 245 mmol) was added, and the mixture was stirred for 16 hours. The reaction mixture was cooled to room temperature, and water (300 mL), hexane (200 mL) and ethyl acetate (200 mL) were added for partitioning. The aqueous layer was discarded, and the organic layer and precipitated crystals were washed with water (300 mL×2). The organic layer and crystals were recovered. The solvent was evaporated under reduced pressure. To the residue were added water (150 mL) and acetonitrile (150 mL) to allow crystallization. The crystals were collected by filtration and thoroughly washed with water and acetonitrile to give di(4-docosoxyphenyl)methylamine (28.1 g, 33.7 mmol, 98% vs —OH).

後処理

  1. temperaturethe mixture was refluxed
  2. stirringthe mixture was stirred for 16 hours
  3. temperatureThe reaction mixture was cooled to room temperature
  4. customfor partitioning
  5. customthe organic layer and precipitated crystals
  6. washwere washed with water (300 mL×2)
  7. customThe organic layer and crystals were recovered
  8. customThe solvent was evaporated under reduced pressure
  9. additionTo the residue were added water (150 mL) and acetonitrile (150 mL)
  10. customcrystallization
  11. filtrationThe crystals were collected by filtration
  12. washthoroughly washed with water and acetonitrile

出典と根拠

ORDレコード
ord-1a079cd4ef834509905c6c1633bd19e8
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08722934B2

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