Hydrochloric Acid → 4-Benzyloxy-2-iodo-5-methoxybenzonitrile

HRID 2381231ノート

反応式

HRID 2381231 の反応式
[CH2:1]([O:8][C:9]1[C:17]([O:18][CH3:19])=[CH:16][C:12]([CH:13]=[N:14]O)=[C:11]([I:20])[CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.FC(F)(F)C(OC(=O)C(F)(F)F)=O.Cl>C(OCC)(=O)C.O1CCCC1>[CH2:1]([O:8][C:9]1[C:17]([O:18][CH3:19])=[CH:16][C:12]([C:13]#[N:14])=[C:11]([I:20])[CH:10]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 9845Trifluoroacetic anhydrideHCID 72327488HCID 72327488、化合物

生成物 1

HCID 671104514-Benzyloxy-2-iodo-5-methoxybenzonitrile収率 51.7%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a mixture of 4-benzyloxy-2-iodo-5-methoxybenzaldehyde oxime (reference example 2-1)(20.8 g), triethylamine (22.7 mL) and tetrahydrofuran (181 mL) was added trifluoroacetic anhydride (23 mL) under ice-bath cooling. After stirring at room temperature for an hour, 2 mol/L hydrochloric acid and ethyl acetate were added to the mixture. The organic layer was washed with brine, and dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was triturated with methanol to give the title compound (10.25 g).

後処理

  1. temperaturecooling
  2. washThe organic layer was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was triturated with methanol

出典と根拠

ORDレコード
ord-4a5f0fc68c5f4cd78fffc49007c50fdb
出典データセット
uspto-grants-2012_09
特許番号
US08258162B2

反応ノート

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