Ammonia → HCID 178492429、化合物

HRID 2075946ノート

反応式

HRID 2075946 の反応式
[CH2:1]([O:8][C:9]1[C:18]([O:19][CH3:20])=[CH:17][C:12]([C:13](Cl)=[N:14][OH:15])=[C:11]([I:21])[CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C[N:23](C)C=O.N.C(OCC)(=O)C>O>[CH2:1]([O:8][C:9]1[C:18]([O:19][CH3:20])=[CH:17][C:12]([C:13]([NH:14][OH:15])=[NH:23])=[C:11]([I:21])[CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 222AmmoniaHCID 6228DimethylformamideHCID 8857Ethyl AcetateHCID 866472264-benzyloxy-N-hydroxy-2-iodo-5-methoxy-benzimidoylchloride

生成物 1

HCID 178492429HCID 178492429、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

To a mixture of 4-benzyloxy-N-hydroxy-2-iodo-5-methoxy-benzimidoylchloride and N,N-dimethylformamide (110 mL) was added a 28% ammonia in water (12 mL) under ice-bath cooling. After stirring for 3 hours under ice-bath cooling, water and ethyl acetate were added to the mixture. The separated organic layer was washed with water and brine successively, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was triturated with hexane:diethyl ether=1:4 to give the title compound (9.3 g).

後処理

  1. temperaturecooling
  2. temperaturecooling
  3. washThe separated organic layer was washed with water and brine successively
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was triturated with hexane

出典と根拠

ORDレコード
ord-0aa487be90be4afebf7bf65fe3b0e39d
出典データセット
uspto-grants-2011_04
特許番号
US07923462B2

反応ノート

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