Triphosgene → 8-Methoxy-1H-benzo[d][1,3]oxazine-2,4-dione

HRID 617127노트

반응식

HRID 617127 반응식
[NH2:1][C:2]1[C:10]([O:11][CH3:12])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].Cl[C:14](Cl)([O:16]C(=O)OC(Cl)(Cl)Cl)Cl>O1CCCC1>[CH3:12][O:11][C:10]1[C:2]2[NH:1][C:14]([O:5][C:4](=[O:6])[C:3]=2[CH:7]=[CH:8][CH:9]=1)=[O:16]

참가 물질

4

반응물 2

HCID 94429TriphosgeneHCID 2557202-Amino-3-methoxybenzoic acid

생성물 1

HCID 105596798-Methoxy-1H-benzo[d][1,3]oxazine-2,4-dione

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a chilled (0-5° C.) solution of 30.0 g (0.180 mol) of 2-amino-3-methoxybenzoic acid (Aldrich Chemicals) in 500 mL of tetrahydrofuran was added 17.8 g (0.0600 mol) of triphosgene. A precipitate formed upon addition. The ice bath was removed after 15 minutes, and the reaction mixture was stirred for 1 hour at room temperature. The reaction mixture was poured into 1000 mL of water and stirred for thirty minutes. The product (mp 267-268° C.) was filtered and amounted to 32.9 g.

후처리

  1. customA precipitate formed upon addition
  2. customThe ice bath was removed after 15 minutes
  3. additionThe reaction mixture was poured into 1000 mL of water
  4. stirringstirred for thirty minutes
  5. filtrationThe product (mp 267-268° C.) was filtered

출처 및 근거

ORD 기록
ord-61941d03209842d88305795814a28779
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05948775

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