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Methanol → (S)-tert-Butyl 5-[(3,5-bistrifluoromethylbenzyl)-(2-methyl-2H-tetrazol-5-yl)amino]-7-methyl-8-trifluoromethyl-2,3,4,5-tetrahydrobenzo[b]azepine-1-carboxylate

HRID 507035
ノート
印刷プレビュー

反応式

HRID 507035 の反応式
N(C(OC(C)C)=O)=N[C:3](OC(C)C)=O.[F:15][C:16]([F:58])([F:57])[C:17]1[CH:18]=[C:19]([CH:50]=[C:51]([C:53]([F:56])([F:55])[F:54])[CH:52]=1)[CH2:20][N:21]([C:45]1[N:46]=[N:47][NH:48][N:49]=1)[C@H:22]1[CH2:28][CH2:27][CH2:26][N:25]([C:29]([O:31][C:32]([CH3:35])([CH3:34])[CH3:33])=[O:30])[C:24]2[CH:36]=[C:37]([C:41]([F:44])([F:43])[F:42])[C:38]([CH3:40])=[CH:39][C:23]1=2.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.CO>C1(C)C=CC=CC=1>[F:54][C:53]([F:56])([F:55])[C:51]1[CH:50]=[C:19]([CH:18]=[C:17]([C:16]([F:57])([F:15])[F:58])[CH:52]=1)[CH2:20][N:21]([C:45]1[N:46]=[N:47][N:48]([CH3:3])[N:49]=1)[C@H:22]1[CH2:28][CH2:27][CH2:26][N:25]([C:29]([O:31][C:32]([CH3:34])([CH3:35])[CH3:33])=[O:30])[C:24]2[CH:36]=[C:37]([C:41]([F:42])([F:43])[F:44])[C:38]([CH3:40])=[CH:39][C:23]1=2
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 887MethanolHCID 11776TriphenylphosphineHCID 75555Diisopropyl diazene-1,2-dicarboxylateHCID 59432487(S)-tert-Butyl 5-[(3,5-bistrifluoromethylbenzyl)-(2H-tetrazol-5-yl)amino)-7-methyl-8-trifluoromethyl-2,3,4,5-tetrahydrobenzo[b]azepine-1-carboxylate

生成物 1

HCID 11585492
(S)-tert-Butyl 5-[(3,5-bistrifluoromethylbenzyl)-(2-methyl-2H-tetrazol-5-yl)amino]-7-methyl-8-trifluoromethyl-2,3,4,5-tetrahydrobenzo[b]azepine-1-carboxylate
収率 95%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Add diisopropyl azodicarboxylate (0.56 mL, 3.94 mmol) to a solution of (S)-tert-butyl 5-[(3,5-bistrifluoromethylbenzyl)-(2H-tetrazol-5-yl)amino]-7-methyl-8-trifluoromethyl-2,3,4,5-tetrahydrobenzo[b]azepine-1-carboxylate (2.10 g, 3.29 mmol) and triphenylphosphine (1.03 g, 3.94 mmol) in methanol (0.20 mL, 4.94 mmol) and toluene (30 mL) at 0° C. under nitrogen. Warm the mixture to room temperature and stir for 12 h. Add silica gel, remove the solvents under reduced pressure and purify the residue by column chromatography on silica gel, eluting with ethyl acetate/hexanes (1:3), to provide the title compound as a colorless oil (2.04 g, 95%). APCI MS m/z 653 (M+H)+.

後処理

  1. customAdd silica gel, remove the solvents under reduced pressure
  2. custompurify the residue by column chromatography on silica gel
  3. washeluting with ethyl acetate/hexanes (1:3)

出典と根拠

ORDレコード
ord-e1d5ec225d5f4d6a8600315609b92a60
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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