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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 1350990
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HRID 1350990 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-fb86279a2d2b4bb8956aecc8e19a0d78
출처 데이터셋
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07214715B2

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