Water → HCID 58238629、化合物

HRID 41327ノート

反応式

HRID 41327 の反応式
[CH3:1][O:2][C:3]1[CH:16]=[CH:15][CH:14]=[CH:13][C:4]=1/[N:5]=[CH:6]/[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[Li][C:18]([CH3:21])([CH3:20])[CH3:19].O>C1COCC1.CCCCC>[CH3:19][C:18]([CH3:21])([CH3:20])[CH:6]([NH:5][C:4]1[CH:13]=[CH:14][CH:15]=[CH:16][C:3]=1[O:2][CH3:1])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

参加物

6

反応物 3

HCID 962WaterHCID 178418306HCID 178418306、化合物HCID 178489586HCID 178489586、化合物

生成物 1

HCID 58238629HCID 58238629、化合物収率 93%

試薬・触媒・溶媒 2

HCID 8003Pentane溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-80 °C

実験手順

To a solution of 1.27 g (6.00 mmol) of 9 in 40 mL of THF, 4.20 mL (6.30 mmol) of 1.5 M tBuLi in pentane was added with vigorous stirring at −80° C. The mixture was slowly warmed to room temperature, and then 2 mL of water was added. The resulting mixture was evaporated to dryness. The product was isolated by flash chromatography on silica gel 60 (40-63 um, eluent: from hexanes to hexanes-diethyl ether=40:1, vol.) to yield 1.50 g (93%) of B1.

後処理

  1. temperatureThe mixture was slowly warmed to room temperature
  2. customThe resulting mixture was evaporated to dryness
  3. customThe product was isolated by flash chromatography on silica gel 60 (40-63 um, eluent: from hexanes to hexanes-diethyl ether=40:1, vol.)

出典と根拠

ORDレコード
ord-ab640f051e334e1a82ee542ac64a9fd8
出典データセット
uspto-grants-2013_09
特許番号
US08530593B2

反応ノート

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