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Methyl chloroformate → ST50924908

HRID 2307407
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HRID 2307407 반응식
Cl[C:2]([O:4][CH3:5])=[O:3].[CH2:6]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[CH2:9][CH2:8][NH:7]1.C(N(CC)CC)C>C(Cl)Cl>[CH3:5][O:4][C:2]([N:7]1[CH2:8][CH2:9][C:10]2[C:15](=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH2:6]1)=[O:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6586Methyl chloroformateHCID 70461,2,3,4-TetrahydroisoquinolineHCID 8471Triethylamine

생성물 1

HCID 3441966ST50924908수율 99.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of methyl chloroformate (15.45 mL, 200 mmol) in CH2Cl2 (50 mL) was added to a solution of 1,2,3,4-tetrahydroisoquinoline (13.3 g, 100 mmol) and triethylamine (57 mL, 400 mmol) in CH2Cl2 (200 mL) at 0° C. The reaction mixture was stirred for 3 hours then was quenched with water. The organic layer was separated and washed with water (2×50 mL). The organic layer was then dried over anhydrous magnesium sulfate, filtered and the resultant filtrate was concentrated in vacuo to provide the title compound (19.1 g). The crude material thus obtained was used without further purification.

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후처리

  1. customthen was quenched with water
  2. customThe organic layer was separated
  3. washwashed with water (2×50 mL)
  4. dry with materialThe organic layer was then dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationthe resultant filtrate was concentrated in vacuo

출처 및 근거

ORD 기록
ord-c13effe7e0524f3482a208749a8fa67d
출처 데이터셋
uspto-grants-2004_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06831080B2

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