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Pyridine → (S)-5-[(3,5-Bis-trifluoromethyl-benzyl)-(2-methyl-2H-tetrazol-5-yl)-amino]-7-methyl-8-trifluoromethyl-2,3,4,5-tetrahydro-benzo[b]azepine-1-carboxylic acid 1-ethyl-propyl ester

HRID 507043
ノート
印刷プレビュー

反応式

HRID 507043 の反応式
[CH3:1][CH2:2][CH:3]([OH:6])[CH2:4][CH3:5].[C:7](Cl)(Cl)=[O:8].C1(C)C=CC=CC=1.[F:18][C:19]([F:55])([F:54])[C:20]1[CH:21]=[C:22]([CH:47]=[C:48]([C:50]([F:53])([F:52])[F:51])[CH:49]=1)[CH2:23][N:24]([C:41]1[N:42]=[N:43][N:44]([CH3:46])[N:45]=1)[C@H:25]1[CH2:31][CH2:30][CH2:29][NH:28][C:27]2[CH:32]=[C:33]([C:37]([F:40])([F:39])[F:38])[C:34]([CH3:36])=[CH:35][C:26]1=2.N1C=CC=CC=1>ClCCl>[CH2:2]([CH:3]([O:6][C:7]([N:28]1[CH2:29][CH2:30][CH2:31][C@H:25]([N:24]([CH2:23][C:22]2[CH:47]=[C:48]([C:50]([F:53])([F:52])[F:51])[CH:49]=[C:20]([C:19]([F:18])([F:55])[F:54])[CH:21]=2)[C:41]2[N:42]=[N:43][N:44]([CH3:46])[N:45]=2)[C:26]2[CH:35]=[C:34]([CH3:36])[C:33]([C:37]([F:39])([F:38])[F:40])=[CH:32][C:27]1=2)=[O:8])[CH2:4][CH3:5])[CH3:1]
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

7

反応物 5

HCID 1049PyridineHCID 1140TolueneHCID 6371PhosgeneHCID 114283-PentanolHCID 59432408(S)-(3,5-bistrifluoromethylbenzyl)-(2-methyl-2H-tetrazol-5-yl)-(7-methyl-8-trifluoromethyl-2,3,4,5-tetrahydro-1H-benzo[b]azepin-5-yl)amine

生成物 1

HCID 11707331
(S)-5-[(3,5-Bis-trifluoromethyl-benzyl)-(2-methyl-2H-tetrazol-5-yl)-amino]-7-methyl-8-trifluoromethyl-2,3,4,5-tetrahydro-benzo[b]azepine-1-carboxylic acid 1-ethyl-propyl ester
収率 59%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

反応条件

温度
0 °C

実験手順

To a mixture of pentan-3-ol (0.117 ml, 1.08 mmol) di-isopropyl ethyl amine (0.189 ml, 1.08 mmol) in dichloromethane at 0° C. with 20% phosgene in toluene (0.480 ml, 0.905 mmol). Stir the mixture at 0° C. for 10 minutes, and then warm up to room temperature for an hour. Add a solution of (S)-(3,5-bis-trifluoromethyl-benzyl)-(2-methyl-2H-tetrazol-5-yl)-(7-methyl-8-trifluoromethyl-2,3,4,5-tetrahydro-1H-benzo[b]azepin-5-yl)-amine (0.100 mg, 0.181 mmol) (Example 3, Step 18)) in dichloromethane (1.00 ml) followed by pyridine (0.0730 ml, 0.905 mmol). Continue the reaction at room temperature overnight. Dilute the mixture with dichloromethane (5.05 ml), wash with 1N hydrochloric acid (5.00 ml) and water (3×5.00 ml), dry over Na2SO4 and concentrated. Purify by silica gel chromatography (gradient eluent, 0-25% ethyl acetate in hexane) to provide the titled compound (0.0710 g, 59%). MS (ES+): 667 (M+H).

後処理

  1. temperaturewarm up to room temperature for an hour
  2. customthe reaction at room temperature overnight
  3. washwash with 1N hydrochloric acid (5.00 ml) and water (3×5.00 ml)
  4. dry with materialdry over Na2SO4
  5. concentrationconcentrated
  6. customPurify by silica gel chromatography (gradient eluent, 0-25% ethyl acetate in hexane)

出典と根拠

ORDレコード
ord-81145fc154574cc68e170e60666a0ad2
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07786108B2

反応ノート

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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