Triethylamine → HCID 16039366、化合物

HRID 639284ノート

反応式

HRID 639284 の反応式
[Cl:1][C:2]1[CH:28]=[CH:27][C:5]([O:6][CH2:7][C:8]([N:10]2[C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=3[CH2:14][N:13]3[C:21]([C:24](Cl)=[O:25])=[CH:22][CH:23]=[C:12]3[CH2:11]2)=[O:9])=[CH:4][CH:3]=1.C(N(CC)CC)C.Cl.[CH3:37][C:38]1[C:43]([NH2:44])=[CH:42][CH:41]=[C:40]([C:45]2[CH:50]=[CH:49][CH:48]=[CH:47][C:46]=2[CH3:51])[CH:39]=1>O1CCCC1>[Cl:1][C:2]1[CH:28]=[CH:27][C:5]([O:6][CH2:7][C:8]([N:10]2[C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=3[CH2:14][N:13]3[C:21]([C:24]([NH:44][C:43]4[CH:42]=[CH:41][C:40]([C:45]5[CH:50]=[CH:49][CH:48]=[CH:47][C:46]=5[CH3:51])=[CH:39][C:38]=4[CH3:37])=[O:25])=[CH:22][CH:23]=[C:12]3[CH2:11]2)=[O:9])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 1488202',3-Dimethyl-4-aminobiphenyl hydrochlorideHCID 86607493HCID 86607493、化合物

生成物 1

HCID 16039366HCID 16039366、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred solution of 10-[2-(4-chloro-phenoxy)-acetyl]-10,11-dihydro-5H-benzo[e]pyrrolo[1,2-a][1,4]diazepine-3-carbonyl chloride of step B (0.415 mmol) in anhydrous tetrahydrofuran (3 mL) was added triethylamine (0.829 mmol) and 3,2′-dimethylbiphen-4-ylamine hydrochloride (0.415 mmol). The solution was stirred for 18 hours at ambient temperature. The solvent was evaporated, the residue was taken up in dichloromethane, washed with water, dried over anhydrous sodium sulfate, and evaporated. Chromatography on silica gel using 55:23:22 hexane/ethyl acetate/dichloromethane as eluant gave the title compound as an amorphous solid. This was crystallized from ethyl acetate/hexane to afford 0.17 g of the title product (71% yield), m.p. 159-161° C. MS [(+)ESI, m/z]: 576 [M+H]+ Anal. Calcd for C35H30CIN3O3: C, 72.97; H, 5.25; N, 7.29. Found: C, 72.59; H, 5.28; N, 7.24.

後処理

  1. customThe solvent was evaporated
  2. washwashed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. customevaporated

出典と根拠

ORDレコード
ord-a2536bb5ca904b5db659b6dc7f971f0f
出典データセット
uspto-grants-2010_04
特許番号
US07691848B2

反応ノート

読み込み中…