Triethylamine → HCID 178490652, 화합물

HRID 78521노트

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HRID 78521 반응식
[C:1]([C:5]1[S:9][C:8](=[NH:10])[NH:7][C:6]=1[CH3:11])([CH3:4])([CH3:3])[CH3:2].C(N(CC)CC)C.[Cl:19][C:20]1[CH:21]=[CH:22][C:23]([O:29][CH3:30])=[C:24]([CH:28]=1)[C:25](Cl)=[O:26]>O1CCCC1>[C:1]([C:5]1[S:9]/[C:8](=[N:10]\[C:25](=[O:26])[C:24]2[CH:28]=[C:20]([Cl:19])[CH:21]=[CH:22][C:23]=2[O:29][CH3:30])/[NH:7][C:6]=1[CH3:11])([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 123841765-Chloro-2-methoxybenzoyl chlorideHCID 178433698HCID 178433698, 화합물

생성물 1

HCID 178490652HCID 178490652, 화합물수율 96.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
60 °C

실험 절차

A mixture of 5-tert-butyl-4-methylthiazol-2(3H)-imine (250 mg, 1.5 mmol) in tetrahydrofuran (10 mL) was treated with triethylamine (0.25 mL, 1.8 mmol) and 5-chloro-2-methoxybenzoylchloride (307 mg, 1.5 mmol). The reaction mixture was stirred at 60° C. for 18 hours then concentrated under reduced pressure. The residue was diluted with ethyl acetate and H2O. The organic extract was dried over MgSO4, filtered, concentrated under reduced pressure and dried under vacuum to afford the title compound (490 mg, 96% yield). MS (ESI) m/z 339 (M+H)+.

후처리

  1. concentrationthen concentrated under reduced pressure
  2. additionThe residue was diluted with ethyl acetate and H2O
  3. extractionThe organic extract
  4. dry with materialwas dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customdried under vacuum

출처 및 근거

ORD 기록
ord-2c4bc027392140b2aba9a88c008707d6
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08841334B2

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