Methyl chloroformate → HCID 13575671、化合物

HRID 465023ノート

反応式

HRID 465023 の反応式
[CH3:1][CH:2]1[CH2:6][C:5]2[C:7]([CH3:13])=[CH:8][CH:9]=[C:10]([NH:11][NH2:12])[C:4]=2[O:3]1.C(N(CC)C(C)C)(C)C.Cl[C:24]([O:26][CH3:27])=[O:25]>C1COCC1>[CH3:27][O:26][C:24]([NH:12][NH:11][C:10]1[C:4]2[O:3][CH:2]([CH3:1])[CH2:6][C:5]=2[C:7]([CH3:13])=[CH:8][CH:9]=1)=[O:25]

参加物

5

反応物 3

HCID 6586Methyl chloroformateHCID 81531DiisopropylethylamineHCID 13575670HCID 13575670、化合物

生成物 1

HCID 13575671HCID 13575671、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-5 °C

実験手順

15.6 g of 1E was mixed with 150 ml of THF and 11.3 g of N,N-diisopropylethylamine. The mixture was cooled to -5° C. and 9.1 g of methyl chloroformate was added drop-by-drop to the stirred mixture, stirred at 0° C. for two hours, then poured over ice water and extracted with ether. The extract was dried (MgSO4) and the solvent was evaporated. The residue was column chromatographed on silica gel, using a 1:4:20 v:v:v mixture of tetrahydrofuran, ethyl acetate and hexane as eluent, to give 2-(2,3-dihydro-2,4-dimethylbenzofuran-7-yl)hydrazinecarboxylic acid methyl ester (1F), as a tan solid, m.p.: 90°-92° C.

後処理

  1. extractionextracted with ether
  2. dry with materialThe extract was dried (MgSO4)
  3. customthe solvent was evaporated
  4. customchromatographed on silica gel
  5. additionv:v mixture of tetrahydrofuran, ethyl acetate and hexane as eluent

出典と根拠

ORDレコード
ord-0e30df148e214556a028d39347442c01
出典データセット
uspto-grants-1985_10
特許番号
US04550121

反応ノート

読み込み中…