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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Acetyl chloride → 1-[8-Chloro-1-(3,4,5,6-tetrahydro-2h-[1,2']bipyridinyl-4-yl)-4h,6h-2,3,5,10b-tetraaza-benzo[e]azulen-5-yl]-ethanone dihydrochloride

HRID 2118030
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HRID 2118030 반응식
[C:1]([Cl:4])(=[O:3])[CH3:2].[Cl:5][C:6]1[CH:31]=[CH:30][C:9]2[N:10]3[C:14]([CH2:15][NH:16][CH2:17][C:8]=2[CH:7]=1)=[N:13][N:12]=[C:11]3[CH:18]1[CH2:23][CH2:22][N:21]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][N:25]=2)[CH2:20][CH2:19]1>ClCCl>[ClH:4].[ClH:5].[Cl:5][C:6]1[CH:31]=[CH:30][C:9]2[N:10]3[C:14]([CH2:15][N:16]([C:1](=[O:3])[CH3:2])[CH2:17][C:8]=2[CH:7]=1)=[N:13][N:12]=[C:11]3[CH:18]1[CH2:19][CH2:20][N:21]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][N:25]=2)[CH2:22][CH2:23]1
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참가 물질

4

반응물 2

HCID 6367Acetyl chlorideHCID 113264888-Chloro-1-(3,4,5,6-tetrahydro-2h-[1,2']bipyridinyl-4-yl)-5,6-dihydro4h-2,3,5,10b-tetraaza-benzo[e]azulene

생성물 1

HCID 219255551-[8-Chloro-1-(3,4,5,6-tetrahydro-2h-[1,2']bipyridinyl-4-yl)-4h,6h-2,3,5,10b-tetraaza-benzo[e]azulen-5-yl]-ethanone dihydrochloride수율 83.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Acetyl chloride (0.1 ml, 1.4 mmol) was added to an ice cooled solution of the amine of example 4 (200 mg, 0.53 mmol) in dichloromethane (5 ml) and stirred at room temperature for 20 hours. Dichloromethane was evaporated off under reduced pressure and the residue purified by chromatography on silica gel using methanol in dichloromethane (5:95) as eluant. The residue was dissolved in dichloromethane (2 ml) and hydrochloric acid (1M in diethyl ether, 2 ml) was added, and the solvents evaporated under reduced pressure to give the title compound as a brown foam (110 mg).

후처리

  1. customDichloromethane was evaporated off under reduced pressure
  2. customthe residue purified by chromatography on silica gel
  3. dissolutionThe residue was dissolved in dichloromethane (2 ml)
  4. additionhydrochloric acid (1M in diethyl ether, 2 ml) was added
  5. customthe solvents evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-cd6e84855b4042ac8ecfcb269f63e6ce
출처 데이터셋
uspto-grants-2008_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07442795B2

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