2-Bromopropane → HCID 90034214、化合物

HRID 1487962ノート

反応式

HRID 1487962 の反応式
[NH:1]1[C:5]2[CH2:6][CH2:7][NH:8][CH2:9][CH2:10][C:4]=2[N:3]=[C:2]1[C:11]1[C:12]([CH3:22])=[CH:13][C:14]([CH3:21])=[C:15]([CH:20]=1)[C:16]([O:18][CH3:19])=[O:17].Br[CH:24]([CH3:26])[CH3:25].C(N(CC)C(C)C)(C)C>CN(C)C=O.C(OCC)(=O)C>[CH:24]([N:8]1[CH2:7][CH2:6][C:5]2[N:1]=[C:2]([C:11]3[C:12]([CH3:22])=[CH:13][C:14]([CH3:21])=[C:15]([CH:20]=3)[C:16]([O:18][CH3:19])=[O:17])[NH:3][C:4]=2[CH2:10][CH2:9]1)([CH3:26])[CH3:25]

参加物

6

反応物 3

HCID 63582-BromopropaneHCID 81531DiisopropylethylamineHCID 90066696HCID 90066696、化合物2 回

生成物 1

HCID 90034214HCID 90034214、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

Into a 100-mL round-bottom flask, was placed methyl 5-(1,4,5,6,7,8-hexahydroimidazo[4,5-d]azepin-2-yl)-2,4-dimethylbenzoate (compound 83.4, 347 mg, 0.84 mmol), 2-bromopropane (790 μL, 8.40 mmol), N,N-diisopropylethylamine (1.46 mL, 8.4 mmol) in N,N-dimethylformamide (5 mL). The solution was stirred for 4 h at 80° C., then cooled to room temperature. The resulting solution was diluted with ethyl acetate (50 mL) and washed with brine (4×20 mL), dried (Na2SO4), filtered, and concentrated under reduced pressure to yield 0.22 g (crude) of the title compound as brown oil.

後処理

  1. customInto a 100-mL round-bottom flask, was placed
  2. temperaturecooled to room temperature
  3. washwashed with brine (4×20 mL)
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-791f12eaa8134b928d086837547da181
出典データセット
uspto-grants-2016_08
特許番号
US09428502B2

反応ノート

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