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Dimethylformamide → (S)-3-methyl-2-{4'-[(5-trifluoromethyl-benzothiazole-2-carbonyl)-amino]-biphenyl-4-sulfonylamino}-butyric acid tert-butyl ester

HRID 29450
ノート
印刷プレビュー

反応式

HRID 29450 の反応式
[Na+].[F:2][C:3]([F:17])([F:16])[C:4]1[CH:5]=[CH:6][C:7]2[S:11][C:10]([C:12]([O-:14])=O)=[N:9][C:8]=2[CH:15]=1.[C:18]([O:22][C:23](=[O:45])[C@@H:24]([NH:28][S:29]([C:32]1[CH:37]=[CH:36][C:35]([C:38]2[CH:43]=[CH:42][C:41]([NH2:44])=[CH:40][CH:39]=2)=[CH:34][CH:33]=1)(=[O:31])=[O:30])[CH:25]([CH3:27])[CH3:26])([CH3:21])([CH3:20])[CH3:19].F[P-](F)(F)(F)(F)F.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1.CN(C=O)C>[Cl-].[Na+].O>[C:18]([O:22][C:23](=[O:45])[C@@H:24]([NH:28][S:29]([C:32]1[CH:33]=[CH:34][C:35]([C:38]2[CH:39]=[CH:40][C:41]([NH:44][C:12]([C:10]3[S:11][C:7]4[CH:6]=[CH:5][C:4]([C:3]([F:2])([F:17])[F:16])=[CH:15][C:8]=4[N:9]=3)=[O:14])=[CH:42][CH:43]=2)=[CH:36][CH:37]=1)(=[O:31])=[O:30])[CH:25]([CH3:27])[CH3:26])([CH3:20])([CH3:21])[CH3:19]
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 6228DimethylformamideHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 10525284(S)-2-(4'-amino-biphenyl-4-sulfonylamino)-3-methyl-butyric acid tert-butyl esterHCID 687139225-Trifluoromethyl-benzothiazole-2-carboxylic acid sodium salt

生成物 1

HCID 68714729
(S)-3-methyl-2-{4'-[(5-trifluoromethyl-benzothiazole-2-carbonyl)-amino]-biphenyl-4-sulfonylamino}-butyric acid tert-butyl ester
収率 37.4%

試薬・触媒・溶媒 1

HCID 57417360Sodium chloride; water溶媒

実験手順

To 5-trifluoromethyl-benzothiazole-2-carboxylic acid sodium salt (260 mg, 0.97 mmol) was added (S)-2-(4′-amino-biphenyl-4-sulfonylamino)-3-methyl-butyric acid tert-butyl ester (469 mg, 1.2 eq), BOP (515 mg, 1.2 eq) and 5 mL of DMF. The mixture was stirred at room temperature overnight. The reaction mixture was poured into brine, and extracted with ethyl acetate. The combined organic layers were washed with brine and water. Removal of solvent gave the crude product, which was purified by column chromatography on silica gel to give 230 mg of (S)-3-methyl-2-{4′-[(5-trifluoromethyl-benzothiazole-2-carbonyl)-amino]-biphenyl-4-sulfonylamino}-butyric acid tert-butyl ester as a white solid.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe combined organic layers were washed with brine and water
  3. customRemoval of solvent
  4. customgave the crude product, which
  5. customwas purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-a8de0e0a6e7a45f6aadfad65a8312bc2
出典データセット
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07420001B2

反応ノート

読み込み中…

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