Dimethylamine → 2-(2-Iodo-5-methoxyphenyl)-N,N-dimethylacetamide

HRID 1087848

반응식

HRID 1087848 반응식
C(Cl)(=O)C(Cl)=O.[I:7][C:8]1[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[CH:10][C:9]=1[CH2:16][C:17]([OH:19])=O.[CH3:20][NH:21][CH3:22].C(Cl)Cl>C1(C)C=CC=CC=1.CN(C=O)C>[CH3:20][N:21]([CH3:22])[C:17](=[O:19])[CH2:16][C:9]1[CH:10]=[C:11]([O:14][CH3:15])[CH:12]=[CH:13][C:8]=1[I:7]

참가 물질

7

반응물 4

HCID 674DimethylamineHCID 6344DichloromethaneHCID 65578Oxalyl chlorideHCID 8200712-(2-Iodo-5-methoxyphenyl)acetic acid

생성물 1

HCID 140254972-(2-Iodo-5-methoxyphenyl)-N,N-dimethylacetamide

시약·촉매·용매 2

HCID 1140Toluene용매HCID 6228Dimethylformamide용매

실험 절차

A 16.7 g (0.19 mole) sample of oxalyl chloride was added dropwise at 0° C. to a solution of 50.0 g (0.17 mole) of 2-iodo-5-methoxybenzeneacetic acid in 310 ml dry toluene and 31.7 ml of DMF. The mixture was allowed to warm to room temperature and stir for 16 hours. The solution was cooled to 0° C. and dimethylamine gas was admitted until the mixture was strongly basic. The mixture was allowed to warm to room temperature and stir for three hours and methylene chloride was added. The organic layer was washed with water, dilute hydrochloric acid, and sodium hydroxide. The organic layer was dried with MgSO4 and evaporated in vacuo to give 54.2 g of N,N-dimethyl-2-iodo-5-methoxybenzeneacetamide, mp 86°-89° C.

후처리

  1. temperatureThe solution was cooled to 0° C.
  2. temperatureto warm to room temperature
  3. stirringstir for three hours
  4. washThe organic layer was washed with water, dilute hydrochloric acid, and sodium hydroxide
  5. dry with materialThe organic layer was dried with MgSO4
  6. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-7859d13b0a9a4139b7e32a23c9bfb489
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04960798

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