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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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tert-Butyl (3-hydroxypropyl)methylcarbamate → 2-Chloro-5-[3-[3-(methylamino)propoxy]propyl]-N-(tricyclo[3.3.1.13,7]dec-1-ylmethyl)benzamide, dihydrochloride salt

HRID 719653
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반응식

HRID 719653 반응식
CC(OC(=O)[N:7]([CH2:9][CH2:10][CH2:11][OH:12])[CH3:8])(C)C.[Cl:14][C:15]1[CH:34]=[CH:33][C:32]([CH2:35][CH2:36][CH2:37]I)=[CH:31][C:16]=1[C:17]([NH:19][CH2:20][C:21]12[CH2:30][CH:25]3[CH2:26][CH:27]([CH2:29][CH:23]([CH2:24]3)[CH2:22]1)[CH2:28]2)=[O:18]>ClCCl.FC(F)(F)C([O-])=O.[Ag+]>[ClH:14].[ClH:14].[Cl:14][C:15]1[CH:34]=[CH:33][C:32]([CH2:35][CH2:36][CH2:37][O:12][CH2:11][CH2:10][CH2:9][NH:7][CH3:8])=[CH:31][C:16]=1[C:17]([NH:19][CH2:20][C:21]12[CH2:30][CH:25]3[CH2:26][CH:27]([CH2:29][CH:23]([CH2:24]3)[CH2:22]1)[CH2:28]2)=[O:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 10375241tert-Butyl (3-hydroxypropyl)methylcarbamateHCID 689262302-Chloro-5-(3-iodopropyl)-N-(tricyclo[3.3.1.13,7]dec-1-ylmethyl)benzamide

생성물 1

HCID 101181242-Chloro-5-[3-[3-(methylamino)propoxy]propyl]-N-(tricyclo[3.3.1.13,7]dec-1-ylmethyl)benzamide, dihydrochloride salt수율 7.3%

시약·촉매·용매 2

HCID 76299Silver trifluoroacetate촉매
HCID 6344
Dichloromethane
용매

실험 절차

Silver trifluoroacetate (0.7 g, 3.2 mmol) was added to 1,1-dimethylethyl (3-hydroxypropyl)methyl carbamic acid (1.8 g, 9.5 mmol), [Synth. Commun. (1995), 25(14), 2135–43] in dichloromethane (20 ml). After 10 min. 2-chloro-5-(3-iodopropyl)-N-(tricyclo[3.3.1.13,7]dec-1-ylmethyl) benzamide (1.0 g, Example 70a) was added and the mixture was stirred for 24 h The resulting mixture was washed with water and concentrated. Treatment with 4M hydrochloric acid in 1,4-dioxane/methanol, concentration and purification by RPHPLC gave the title compound (26 mg) as a white solid.

후처리

  1. washwas washed with water
  2. concentrationconcentrated
  3. concentrationTreatment with 4M hydrochloric acid in 1,4-dioxane/methanol, concentration and purification by RPHPLC

출처 및 근거

ORD 기록
ord-3dd95ca2e752426eb491dbe5879f154a
출처 데이터셋
uspto-grants-2006_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07132457B2

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