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Triethylamine → HCID 178488147, 화합물

HRID 1817286
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HRID 1817286 반응식
[Na].[CH3:2][O:3][C:4]1[CH:25]=[CH:24][C:7]2[NH:8][C:9]([S:11]([CH2:13][C:14]3[C:19]([CH3:20])=[C:18]([O:21][CH3:22])[C:17]([CH3:23])=[CH:16][N:15]=3)=[O:12])=[N:10][C:6]=2[CH:5]=1.C([C@](C([O-])=O)(O)[C@](CC)(O)C([O-])=O)C.C(N(CC)CC)C.C(O)(=O)[C@H](C1C=CC=CC=1)O>CC(C)=O.CC(C)[O-].[Ti+4].CC(C)[O-].CC(C)[O-].CC(C)[O-]>[CH3:23][C:17]1[CH:16]=[N:15][C:14]([CH2:13][S+:11]([O-:12])[C:9]2[NH:8][C:7]3[CH:24]=[CH:25][C:4]([O:3][CH3:2])=[CH:5][C:6]=3[N:10]=2)=[C:19]([CH3:20])[C:18]=1[O:21][CH3:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 439616(S)-mandelic acidHCID 29414049diethyl-D-tartarateHCID 178488156HCID 178488156, 화합물

생성물 1

HCID 178488147HCID 178488147, 화합물

시약·촉매·용매 2

HCID 11026Titanium isopropoxide촉매
HCID 180
Acetone
용매
2회

실험 절차

The procedure was carried out as described in Raju et al, Organic Process Research & Development 2006, 10, 33-35, which is hereby incorporated by reference in its entirety. To a suspension of omeprazole sodium salt (5.53 g, 15.1 mmol, 1 equiv) in acetone (60 mL), were added a solution of diethyl-D-tartrate (3.1 g, 15.1 mol, 1 equiv) in acetone (3 mL), titanium (IV) isopropoxide (2.14 g, 7.55 mmol, 0.5 equiv) and triethylamine (4.75 g, 45.3 mmol, 3 equiv) at 35-40° C. To the resulting homogeneous solution was added L-(+)-mandelic acid (2.64 g, 17.4 mmol, 1.15 equiv). The mixture was cooled to ambient temperature and stirred for about 1-2 hours. The precipitate was filtered, washed with acetone (30 mL), and dried under reduced pressure to afford esomeprazole mandalate salt.

후처리

  1. filtrationThe precipitate was filtered
  2. washwashed with acetone (30 mL)
  3. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-a331987f5f5c4b39ac0b2dead2adf1b7
출처 데이터셋
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07598273B2

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