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

Triethylamine → HCID 89689438、化合物

HRID 710256
ノート
印刷プレビュー

反応式

HRID 710256 の反応式
[NH2:1][C@H:2]([C:5]1[CH:10]=[CH:9][C:8]([F:11])=[CH:7][CH:6]=1)[CH2:3][OH:4].[C:12]([O:16][C:17]([N:19]1[CH2:24][CH2:23][O:22][C@@H:21]([C:25]2[CH:33]=[CH:32][C:28]([C:29](O)=[O:30])=[CH:27][CH:26]=2)[CH2:20]1)=[O:18])([CH3:15])([CH3:14])[CH3:13].C(N=C=NCCCN(C)C)C.C(N(CC)CC)C>CN(C)C1C=CN=CC=1.ClCCl>[F:11][C:8]1[CH:9]=[CH:10][C:5]([C@@H:2]([NH:1][C:29]([C:28]2[CH:27]=[CH:26][C:25]([C@@H:21]3[O:22][CH2:23][CH2:24][N:19]([C:17]([O:16][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:18])[CH2:20]3)=[CH:33][CH:32]=2)=[O:30])[CH2:3][OH:4])=[CH:6][CH:7]=1
参加物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 8471TriethylamineHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 10583003(R)-2-Amino-2-(4-fluorophenyl)ethanolHCID 668420684-(1,1-Dimethylethyl) (2S)-2-(4-carboxyphenyl)-4-morpholinecarboxylate

生成物 1

HCID 89689438HCID 89689438、化合物収率 51.1%

試薬・触媒・溶媒 2

HCID 14284
4-(Dimethylamino)pyridine
触媒
HCID 6344Dichloromethane溶媒

実験手順

A mixture of (R)-2-amino-2-(4-fluorophenyl)ethanol (68.6 mg, 0.44 mmol), (S)-4-(4-(tert-butoxycarbonyl)morpholin-2-yl)benzoic acid [CAS 1131220-40-0], (136 mg, 0.44 mmol), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide (170 mg, 0.88 mmol), 4-dimethylaminopyridine (54.0 mg, 0.44 mmol) and triethylamine (179 mg, 0.25 ml, 1.77 mmol) in dichloromethane (9 ml) was stirred at room temperature overnight. The reaction was quenched by addition of 1M citric acid solution (5 ml). The organic layer was separated, washed with sodium bicarbonate saturated solution (5 ml), dried over MgSO4 and evaporated. The crude material was purified by flash chromatography (silica gel, gradient heptane/ethyl acetate), to give a white foam (100 mg, 51%), MS (ISP): 445.4 (100%, [M-tBu+H]+), 389.3 (29%, [M+H]+).

後処理

  1. customThe reaction was quenched by addition of 1M citric acid solution (5 ml)
  2. customThe organic layer was separated
  3. washwashed with sodium bicarbonate saturated solution (5 ml)
  4. dry with materialdried over MgSO4
  5. customevaporated
  6. customThe crude material was purified by flash chromatography (silica gel, gradient heptane/ethyl acetate)

出典と根拠

ORDレコード
ord-990fb4092e274f39a6c3fa5c5c5c070b
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09181230B2

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