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Phosgene → HCID 85868104, 화합물

HRID 1182113
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HRID 1182113 반응식
[C:1]([Cl:4])(Cl)=[O:2].[CH3:5][O:6][C:7]1[CH:8]=[C:9](NC)[CH:10]=[C:11]([O:13][CH3:14])[CH:12]=1.[CH2:17]([N:19](CC)CC)C>C1(C)C=CC=CC=1.ClCCl>[CH3:14][O:13][C:11]1[CH:10]=[C:9]([CH2:17][NH:19][C:1]([Cl:4])=[O:2])[CH:8]=[C:7]([O:6][CH3:5])[CH:12]=1
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참가 물질

6

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HCID 6371PhosgeneHCID 8471TriethylamineHCID 145235363,5-Dimethoxy-N-methylbenzenamine

생성물 1

HCID 85868104HCID 85868104, 화합물

시약·촉매·용매 2

HCID 1140Toluene용매HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

A solution of phosgene (11.6 mmol) in toluene (6 ml) is diluted with dichloromethane (15 ml) and cooled to 0° C. To this is added a solution of (3,5-Dimethoxy-phenyl)-methyl-amine (1.67 g, 10 mmol) and triethylamine (1.78 ml, 14.0 mmol) in dichloromethane (5 ml) slowly over 30 minutes, and the reaction mixture allowed to warm to ambient temperature with stirring over 2 hours. After stirring at ambient temperature for a further 2 hours, the reaction mixture is partitioned between ether and 1M hydrochloric acid solution. The ether phase is washed with brine, dried over magnesium sulphate and evaporated to afford (3,5-Dimethoxy-phenyl)methyl-carbamoyl chloride as a white solid.

후처리

  1. temperatureto warm to ambient temperature
  2. stirringAfter stirring at ambient temperature for a further 2 hours
  3. customthe reaction mixture is partitioned between ether and 1M hydrochloric acid solution
  4. washThe ether phase is washed with brine
  5. dry with materialdried over magnesium sulphate
  6. customevaporated

출처 및 근거

ORD 기록
ord-383c105e13fd49cda3432c6f712c77c1
출처 데이터셋
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07288537B2

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