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Acetic Acid → (S)-5-(3-fluoro-5-trifluoromethyl-benzylamino)-7-methyl-8-trifluoromethyl-2,3,4,5-tetrahydro-benzo[b]azepine-1-carboxylic acid tert-butyl ester

HRID 507176
ノート
印刷プレビュー

反応式

HRID 507176 の反応式
C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[F:15][C:16]1[CH:17]=[C:18]([CH:21]=[C:22]([C:24]([F:27])([F:26])[F:25])[CH:23]=1)[CH:19]=O.C(O)(=O)C.[NH2:32][C@H:33]1[CH2:39][CH2:38][CH2:37][N:36]([C:40]([O:42][C:43]([CH3:46])([CH3:45])[CH3:44])=[O:41])[C:35]2[CH:47]=[C:48]([C:52]([F:55])([F:54])[F:53])[C:49]([CH3:51])=[CH:50][C:34]1=2.C(=O)(O)[O-].[Na+]>ClC(Cl)C>[C:43]([O:42][C:40]([N:36]1[CH2:37][CH2:38][CH2:39][C@H:33]([NH:32][CH2:19][C:18]2[CH:21]=[C:22]([C:24]([F:27])([F:26])[F:25])[CH:23]=[C:16]([F:15])[CH:17]=2)[C:34]2[CH:50]=[C:49]([CH3:51])[C:48]([C:52]([F:55])([F:53])[F:54])=[CH:47][C:35]1=2)=[O:41])([CH3:46])([CH3:45])[CH3:44]
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 5

HCID 176Acetic AcidHCID 516892Sodium BicarbonateHCID 6056863-Fluoro-5-(trifluoromethyl)benzaldehydeHCID 5049666Sodium triacetoxyborohydrideHCID 59432516(S)-tert-Butyl 5-amino-7-methyl-8-(trifluoromethyl)-2,3,4,5-tetrahydro-1H-benzo[b]azepine-1-carboxylate

生成物 1

HCID 59432467
(S)-5-(3-fluoro-5-trifluoromethyl-benzylamino)-7-methyl-8-trifluoromethyl-2,3,4,5-tetrahydro-benzo[b]azepine-1-carboxylic acid tert-butyl ester
収率 98%

試薬・触媒・溶媒 1

HCID 63651,1-Dichloroethane溶媒

実験手順

Add sodium triacetoxyborohydride (0.40 g, 1.89 mmol) to a mixture of 3-fluoro-5-trifluoromethyl benzaldehyde (0.096 mL, 0.69 mmol), acetic acid (0.030 mL, 0.625 mmol)) and (S)-tert-Butyl 5-amino-7-methyl-8-trifluoromethyl-2,3,4,5-tetrahydrobenzo[b]azepine-1-carboxylate (Example 3, Step 13) (0.215 g, 0.63 mmol) in dichloroethane (3.0 mL). Stir the mixture at room temperature under an atmosphere of nitrogen for 20 h. Add a saturated solution of sodium bicarbonate, separate the layers and extract the aqueous layer with dichloromethane. Dry the combined organic layers over anhydrous sodium sulfate, filter, and remove the solvent under reduced pressure. Purify the residue by flash chromatography, eluting with hexanes/ethyl acetate (gradient eluent, 0-30% ethyl acetate in hexane), to afford the title compound (0.32 g, 98%). MS (ES+): 521 (M+H).

後処理

  1. customseparate the layers
  2. extractionextract the aqueous layer with dichloromethane
  3. dry with materialDry the combined organic layers over anhydrous sodium sulfate
  4. filtrationfilter
  5. customremove the solvent under reduced pressure
  6. customPurify the residue by flash chromatography
  7. washeluting with hexanes/ethyl acetate (gradient eluent, 0-30% ethyl acetate in hexane)

出典と根拠

ORDレコード
ord-b079fc63019947bcb4c3b95125aca588
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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