1,8-Diazabicyclo(5.4.0)undec-7-ene → HCID 773523、化合物

HRID 1084985ノート

反応式

HRID 1084985 の反応式
Br[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][S:9]([CH3:12])(=[O:11])=[O:10].C1CCN2C(=NCCC2)CC1.CCCCCC.[C:30](OCC)(=[O:32])C>CO.N1C2C(=CC=C3C=2N=CC=C3)C=CC=1>[CH3:12][S:9]([NH:8][C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=1[O:32][CH3:30])(=[O:11])=[O:10]

参加物

6

反応物 3

HCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 3629878N-(2-bromophenyl)methanesulfonamideHCID 21226206Ethyl acetate hexane

生成物 1

HCID 773523HCID 773523、化合物収率 82%

試薬・触媒・溶媒 2

HCID 13181,10-Phenanthroline触媒HCID 887Methanol溶媒

実験手順

2.50 g of 2-bromo-1-methanesulfonylaminobenzene was added to a solution containing 1.52 g of DBU, 85 g of cupric chloride dihydrate, and 90 mg of 1,10-phenanthroline in 40 ml of methanol, and the mixture was heated under reflux for 5 hours. After the temperature was brought to room temperature, the reaction mixture was treated in a usual manner, and crystallization was effected from n-hexane/ethyl acetate, to produce 1.64 g (yield: 82%) of the desired compound.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 5 hours
  3. customwas brought to room temperature
  4. additionthe reaction mixture was treated in a usual manner, and crystallization

出典と根拠

ORDレコード
ord-f955efc499074a4c93bdf5c511463e13
出典データセット
uspto-grants-1991_04
特許番号
US05006660

反応ノート

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