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Trityl chloride → 4-(tert-butoxycarbonylaminomethyl)-5-(tritylamino)-1-[2-(trityloxy)ethyl]-1H-pyrazole

HRID 349579
ノート
印刷プレビュー

反応式

HRID 349579 の反応式
[NH2:1][C:2]1[N:6]([CH2:7][CH2:8][OH:9])[N:5]=[CH:4][C:3]=1[CH2:10][NH:11][C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13].[C:19]1([C:25](Cl)([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.C(N([CH2:44][CH3:45])CC)C>CN(C)C=O.C(OCC)(=O)C>[C:15]([O:14][C:12]([NH:11][CH2:10][C:3]1[CH:4]=[N:5][N:6]([CH2:7][CH2:8][O:9][C:25]([C:45]2[CH:44]=[CH:37][CH:32]=[CH:33][CH:34]=2)([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[C:2]=1[NH:1][C:25]([C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1)([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)=[O:13])([CH3:18])([CH3:17])[CH3:16]
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

6

反応物 3

HCID 6456Trityl chlorideHCID 8471TriethylamineHCID 179619715-amino-4-(tert-butoxycarbonylaminomethyl)-1-(2-hydroxyethyl)-1H-pyrazole

生成物 1

HCID 179620244-(tert-butoxycarbonylaminomethyl)-5-(tritylamino)-1-[2-(trityloxy)ethyl]-1H-pyrazole

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒
HCID 8857
Ethyl Acetate
溶媒

反応条件

温度
70 °C

実験手順

To a solution of 5-amino-4-(tert-butoxycarbonylaminomethyl)-1-(2-hydroxyethyl)-1H-pyrazole (243 g) in N,N-dimethylformamide (1.82 L) was added triphenylmethyl chloride (581 g), triethylamine (452 ml) and N,N-dimethylaminopyridine (9.91 g) successively. The reaction mixture was stirred at 70° C. overnight. After cooling to room temperature, the reaction mixture was diluted with ethyl acetate, washed with water (twice) and brine, dried over magnesium sulfate and filtered. The filtrate was evaporated in vacuo. The residue was purified by silica gel column chromatography to give 4-(tert-butoxycarbonylaminomethyl)-5-(tritylamino)-1-[2-(trityloxy)ethyl]-1H-pyrazole, which was crystallized from diisopropyl ether/hexane (1:2). The resulting crystals were collected by filtration on a glass filter, washed with diisopropyl ether/hexane (1:2) and dried in vacuo to give the objective compound (480 g).

後処理

  1. temperatureAfter cooling to room temperature
  2. washwashed with water (twice) and brine
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. customThe filtrate was evaporated in vacuo
  6. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-1369a873a20e4731a5b8e89b88d82769
出典データセット
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07179801B2

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