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1,2-Dichloroethane → N1-{(1S,2R)-1-benzyl-2-hydroxy-3-[(3-methoxybenzyl)amino]propyl}-N3,N3-dipropyl-5-(3-thienyl)isophthalamide hydrochloride

HRID 348831
ノート
印刷プレビュー

反応式

HRID 348831 の反応式
[CH2:1]([N:4]([CH2:21][CH2:22][CH3:23])[C:5]([C:7]1[CH:8]=[C:9]([CH:13]=[C:14]([C:16]2[CH:20]=[CH:19][S:18][CH:17]=2)[CH:15]=1)[C:10]([OH:12])=O)=[O:6])[CH2:2][CH3:3].FC(F)(F)C(O)=O.[NH2:31][C@@H:32]([CH2:46][C:47]1[CH:52]=[C:51](F)[CH:50]=[C:49](F)[CH:48]=1)[C@H:33]([OH:45])[CH2:34][NH:35][CH2:36][C:37]1[CH:42]=[CH:41][CH:40]=[C:39]([O:43][CH3:44])[CH:38]=1.C1C=CC2N(O)N=NC=2C=1.C(N(CC)CC)C.C(Cl)C[Cl:74]>CN(C=O)C.O>[ClH:74].[CH2:46]([C@H:32]([NH:31][C:10](=[O:12])[C:9]1[CH:13]=[C:14]([C:16]2[CH:20]=[CH:19][S:18][CH:17]=2)[CH:15]=[C:7]([C:5]([N:4]([CH2:21][CH2:22][CH3:23])[CH2:1][CH2:2][CH3:3])=[O:6])[CH:8]=1)[C@H:33]([OH:45])[CH2:34][NH:35][CH2:36][C:37]1[CH:42]=[CH:41][CH:40]=[C:39]([O:43][CH3:44])[CH:38]=1)[C:47]1[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=1
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 111,2-DichloroethaneHCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 210857863-[(Dipropylamino)carbonyl]-5-(3-thienyl)benzoic acidHCID 69869154(2R,3S)-3-amino-4-(3,5-difluorophenyl)-1-[(3-methoxybenzyl)amino]-2-butanol Trifluoroacetate

生成物 1

HCID 68608779
N1-{(1S,2R)-1-benzyl-2-hydroxy-3-[(3-methoxybenzyl)amino]propyl}-N3,N3-dipropyl-5-(3-thienyl)isophthalamide hydrochloride

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 3-[(dipropylamino)carbonyl]-5-(3-thienyl)benzoic acid (IX–L, step 4, 0.26 g, 0.79 mmol), (2R,3S)-3-amino-1-[(3-methoxybenzyl)amino]-4-phenyl-2-butanol dihydrochloride (VIII, 0.26 g, 0.71 mmol), HOBt (0.16 g, 1.18 mmol), and triethylamine (0.44 mL, 3.15 mmol) in DMF (4 mL) is stirred at 20–25 degrees C. for 10 minutes EDC (0.23 g, 1.18 mmol) is added and the reaction mixture is stirred for 4 hours. The reaction mixture is diluted with water and extracted with ethyl acetate. The organic phase is washed with hydrochloric acid (1 N), water, and saline, dried over magnesium sulfate and concentrated under reduced pressure. Recrystallization (methylene chloride/hexanes, 1/1) gives the title compound, mp=199–201 degrees C.; IR (KBr): 3278, 2961, 2874 and 2837 cm−1; ESI-MS (m/z) [M+H]+=614.

後処理

  1. stirringthe reaction mixture is stirred for 4 hours
  2. extractionextracted with ethyl acetate
  3. washThe organic phase is washed with hydrochloric acid (1 N), water, and saline
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customRecrystallization (methylene chloride/hexanes, 1/1)

出典と根拠

ORDレコード
ord-1245a5c3407947af8acc4859286f7853
出典データセット
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07176242B2

反応ノート

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