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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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[7-(5,6-Dihydro-[1,4]dioxin-2-yl)-4-methoxy-benzothiazol-2-yl]-carbamic acid ethyl ester → (+)-(7-[1,4]Dioxan-2-yl-4-methoxy-benzothiazol-2-yl)-carbamic acid ethyl ester

HRID 985801
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HRID 985801 반응식
[CH2:1]([O:3][C:4](=[O:23])[NH:5][C:6]1[S:7][C:8]2[C:14]([C:15]3[O:16][CH2:17][CH2:18][O:19][CH:20]=3)=[CH:13][CH:12]=[C:11]([O:21][CH3:22])[C:9]=2[N:10]=1)[CH3:2].[H][H]>O1CCOCC1.C(O)(=O)C.[Pd]>[CH2:1]([O:3][C:4](=[O:23])[NH:5][C:6]1[S:7][C:8]2[C:14]([CH:15]3[CH2:20][O:19][CH2:18][CH2:17][O:16]3)=[CH:13][CH:12]=[C:11]([O:21][CH3:22])[C:9]=2[N:10]=1)[CH3:2]
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참가 물질

6

반응물 2

HCID 86594649[7-(5,6-Dihydro-[1,4]dioxin-2-yl)-4-methoxy-benzothiazol-2-yl]-carbamic acid ethyl esterHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 86594650(+)-(7-[1,4]Dioxan-2-yl-4-methoxy-benzothiazol-2-yl)-carbamic acid ethyl ester수율 62.1%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 176Acetic Acid용매
HCID 31275
1,4-Dioxane
용매

실험 절차

To a stirred solution of 12.0 g (35.7 mmol) [7-(5,6-dihydro-[1,4]dioxin-2-yl)-4-methoxy-benzothiazol-2-yl]-carbamic acid ethyl ester in 600 ml dioxane and 12 ml acetic acid was added 12 g of 10% palladium on charcoal and the mixture was then stirred for 48 h at room temperature under a 10 bar atmosphere of hydrogen. The mixture was then filtered, washing with dioxane, and the filtrate concentrated in vacuo. Flash chromatography (1/1 acetone/dichloromethane) followed by trituration in ether and hexane afforded 7.50 g (62%) (±)-(7-[1,4]dioxan-2-yl-4-methoxy-benzothiazol-2-yl)-carbamic acid ethyl ester as a white solid. ES-MS m/e (%): 339 (M+H+, 100).

후처리

  1. filtrationThe mixture was then filtered
  2. washwashing with dioxane
  3. concentrationthe filtrate concentrated in vacuo

출처 및 근거

ORD 기록
ord-b1553d3a7e5444349e884241f3658024
출처 데이터셋
uspto-grants-2005_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06872833B2

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