N-Ethoxymethanamine → HCID 14011488, 화합물

HRID 246991노트

반응식

HRID 246991 반응식
[CH3:1][C:2]1([CH3:21])[CH2:6][C:5]2[CH:7]=[C:8]([O:11][C:12]3[CH:17]=[CH:16][C:15]([N:18]=[C:19]=[O:20])=[CH:14][CH:13]=3)[CH:9]=[CH:10][C:4]=2[O:3]1.[CH3:22][NH:23][O:24][CH2:25][CH3:26]>C1(C)C=CC=CC=1>[CH3:1][C:2]1([CH3:21])[CH2:6][C:5]2[CH:7]=[C:8]([O:11][C:12]3[CH:17]=[CH:16][C:15]([NH:18][C:19]([N:23]([O:24][CH2:25][CH3:26])[CH3:22])=[O:20])=[CH:14][CH:13]=3)[CH:9]=[CH:10][C:4]=2[O:3]1

참가 물질

4

반응물 2

HCID 14895678N-EthoxymethanamineHCID 20161048HCID 20161048, 화합물

생성물 1

HCID 14011488HCID 14011488, 화합물수율 96.5%

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

1.8 g of 4-(2,3-dihydro-2,2-dimethyl-5-benzofuranyloxy)phenyl isocyanate was dissolved in 20 ml of toluene, and 2.0 g of N-methyl-O-ethylhydroxylamine dissolved in 5 ml of toluene, was dropwise added thereto over a period of 20 minutes at room temperature. The mixture was stirred at room temperature for 2 hours, and then the solvent was distilled off. The residue was purified by silica gel column chromatography by using a solvent mixture of ethyl acetate/n-hexane=1/4 as the developer, to obtain 2.2 g of compound No. 29 as identified in Table 1.

후처리

  1. additionwas dropwise added
  2. distillationthe solvent was distilled off
  3. customThe residue was purified by silica gel column chromatography
  4. additiona solvent mixture of ethyl acetate/n-hexane=1/4 as the developer

출처 및 근거

ORD 기록
ord-8f23056336404209a1e9e21294f6ca0a
출처 데이터셋
uspto-grants-1987_11
특허 번호
US04705554

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