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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Dimethylamine → 7-Chloro-2-[2-(dimethylamino)ethyl]-2,3-dihydro-4-methyl-1,4-benzoxazepine-5(4H)-thione oxalate hydrate

HRID 1194225
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HRID 1194225 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:11][CH:10]([CH2:12][CH2:13]Cl)[CH2:9][N:8]([CH3:15])[C:7](=[S:16])[C:6]=2[CH:17]=1.[CH3:18][NH:19][CH3:20].[C:21]([OH:26])(=[O:25])[C:22]([OH:24])=[O:23]>C(O)C.C(O)(C)C>[OH2:11].[C:21]([OH:26])(=[O:25])[C:22]([OH:24])=[O:23].[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:11][CH:10]([CH2:12][CH2:13][N:19]([CH3:20])[CH3:18])[CH2:9][N:8]([CH3:15])[C:7](=[S:16])[C:6]=2[CH:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 674DimethylamineHCID 971Oxalic AcidHCID 137263017-Chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepine-5(4H)-thione

생성물 1

HCID 137263387-Chloro-2-[2-(dimethylamino)ethyl]-2,3-dihydro-4-methyl-1,4-benzoxazepine-5(4H)-thione oxalate hydrate

시약·촉매·용매 2

HCID 702Ethanol용매
HCID 3776
Isopropanol
용매

실험 절차

To a solution of 8.0 g (0.027 mole) of 7-chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepine-5(4H)-thione in 50 ml of absolute ethanol was added 6 ml (0.054 mole) of 40% aqueous solution of dimethylamine. The solution was heated in a steel bomb at 90° C. for 14 hr. The ethanol was removed under reduced pressure and the residue was partitioned between chloroform and aqueous sodium hydroxide. The chloroform layer was concentrated to give a viscous yellow oil. The oil was dissolved in isopropyl alcohol and reacted with oxalic acid. The oxalate salt immediately precipitated. The mixture was heated and a small amount of water was added to dissolve the salt. A white crystalline powder was obtained, m.p. 150°-151° C.

후처리

  1. customThe ethanol was removed under reduced pressure
  2. customthe residue was partitioned between chloroform and aqueous sodium hydroxide
  3. concentrationThe chloroform layer was concentrated
  4. customto give a viscous yellow oil
  5. customThe oxalate salt immediately precipitated
  6. temperatureThe mixture was heated
  7. additiona small amount of water was added
  8. dissolutionto dissolve the salt
  9. customA white crystalline powder was obtained

출처 및 근거

ORD 기록
ord-3ac89584dd6142e5a3d030b5bd75a1ef
출처 데이터셋
uspto-grants-1989_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04812565

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