N-Ethoxymethanamine → HCID 14011488、化合物

HRID 246991ノート

反応式

HRID 246991 の反応式
[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

参加物

4

反応物 2

HCID 14895678N-EthoxymethanamineHCID 20161048HCID 20161048、化合物

生成物 1

HCID 14011488HCID 14011488、化合物収率 96.5%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8f23056336404209a1e9e21294f6ca0a
出典データセット
uspto-grants-1987_11
特許番号
US04705554

反応ノート

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