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

HRID 2381231노트

반응식

HRID 2381231 반응식
[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

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 9845Trifluoroacetic anhydrideHCID 72327488HCID 72327488, 화합물

생성물 1

HCID 671104514-Benzyloxy-2-iodo-5-methoxybenzonitrile수율 51.7%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-4a5f0fc68c5f4cd78fffc49007c50fdb
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08258162B2

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