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Triethylamine → (3S,3aR)-2-(3-chloro-4-cyanophenyl)-3-cyclopentyl-N-(2-sulfamoylethyl)-3,3a,4,5-tetrahydro-2H-benzo[g]indazole-7-carboxamide

HRID 505754
ノート
印刷プレビュー

反応式

HRID 505754 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([N:10]2[C@@H:18]([CH:19]3[CH2:23][CH2:22][CH2:21][CH2:20]3)[C@@H:17]3[C:12]([C:13]4[CH:27]=[CH:26][C:25]([C:28]([OH:30])=O)=[CH:24][C:14]=4[CH2:15][CH2:16]3)=[N:11]2)[CH:5]=[CH:6][C:7]=1[C:8]#[N:9].ON1C2C=CC=CC=2N=N1.C(N(CC)CC)C.F[B-](F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2C=CC=CC=2N=N1.[NH2:70][CH2:71][CH2:72][S:73]([NH2:76])(=[O:75])=[O:74]>CN(C)C=O.C(#N)C.O>[Cl:1][C:2]1[CH:3]=[C:4]([N:10]2[C@@H:18]([CH:19]3[CH2:20][CH2:21][CH2:22][CH2:23]3)[C@@H:17]3[C:12]([C:13]4[CH:27]=[CH:26][C:25]([C:28]([NH:70][CH2:71][CH2:72][S:73](=[O:75])(=[O:74])[NH2:76])=[O:30])=[CH:24][C:14]=4[CH2:15][CH2:16]3)=[N:11]2)[CH:5]=[CH:6][C:7]=1[C:8]#[N:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 101263TaurinamideHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 46871935Pf-03882845

生成物 1

HCID 66723212
(3S,3aR)-2-(3-chloro-4-cyanophenyl)-3-cyclopentyl-N-(2-sulfamoylethyl)-3,3a,4,5-tetrahydro-2H-benzo[g]indazole-7-carboxamide
収率 8%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 18373917Acetonitrile--water (1/1)溶媒

実験手順

To a solution of (3S,3aR)-2-(3-chloro-4-cyanophenyl)-3-cyclopentyl-3,3a,4,5-tetrahydro-2H-benzo[g]indazole-7-carboxylic acid, Example 15 (100 mg, 0.24 mmol) in N,N-dimethylformamide (3 mL) was added 1-hydroxybenzotriazole (48 mg, 0.36 mmol), triethylamine (0.07 mL, 0.48 mmol) and O-benzotriazol-1-yl-N,N,N′,N′-tetramethyluronium tetrafluoroborate (115 mg, 0.36 mmol). The solution was stirred for fifteen minutes followed by addition of 2-aminoethanesulfonamide (44 mg, 0.36 mmol). The solution was stirred for twenty hours at ambient temperature. The reaction was partitioned between ethyl acetate and water. The organic layer was washed with water and brine and dried over magnesium sulfate. Chromatography (reverse phase, acetonitrile/water) provided (3S,3aR)-2-(3-chloro-4-cyanophenyl)-3-cyclopentyl-N-(2-sulfamoylethyl)-3,3a,4,5-tetrahydro-2H-benzo[g]indazole-7-carboxamide (yellow solid, 10 mg, 8% yield). LC/MS on 4.6×50 mm C-18 column, tR=5.80 minutes (10 to 90% acetonitrile/water over 6 minutes at 2 mL/minute with detection 254 nm, at 50° C.); ES-MS m/z 526 (M+H).

後処理

  1. stirringThe solution was stirred for twenty hours at ambient temperature
  2. customThe reaction was partitioned between ethyl acetate and water
  3. washThe organic layer was washed with water and brine
  4. dry with materialdried over magnesium sulfate

出典と根拠

ORDレコード
ord-4d6cb10d2d5546b5b4eee9a7795481bf
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07781428B2

反応ノート

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