Ammonia → HCID 19041650, 화합물

HRID 1684013

반응식

HRID 1684013 반응식
[Br:1][C:2]1[CH:27]=[CH:26][C:5]([CH2:6][N:7]2[C:15]3[C:10](=[CH:11][C:12]([O:16][CH3:17])=[CH:13][CH:14]=3)[C:9]([CH2:18][CH:19]([CH3:24])[CH2:20][C:21](O)=[O:22])=[C:8]2[CH3:25])=[CH:4][CH:3]=1.C[N:29](C=O)C.C(Cl)(=O)C(Cl)=O.N>C1C=CC=CC=1.C1COCC1>[Br:1][C:2]1[CH:27]=[CH:26][C:5]([CH2:6][N:7]2[C:15]3[C:10](=[CH:11][C:12]([O:16][CH3:17])=[CH:13][CH:14]=3)[C:9]([CH2:18][CH:19]([CH3:24])[CH2:20][C:21]([NH2:29])=[O:22])=[C:8]2[CH3:25])=[CH:4][CH:3]=1

참가 물질

7

반응물 4

HCID 222AmmoniaHCID 6228DimethylformamideHCID 65578Oxalyl chlorideHCID 98673334-(1-(4-Bromobenzyl)-5-methoxy-2-methyl-1H-indol-3-yl)-3-methylbutanoic acid

생성물 1

HCID 19041650HCID 19041650, 화합물

시약·촉매·용매 2

HCID 241Benzene용매HCID 8028Tetrahydrofuran용매

실험 절차

To the acid of Example 7, Step 6, (600 mg, 1.39 mmol) in benzene (10.0 mL) was added at 0° C. DMF (50 mL) and oxalyl chloride. After a period of 30 min at 0° /C., THF (10.0 mL) was added to the resulting mixture and ammonia gas was bubbled until saturation. The mixture was stirred for 4 h at r.t. The reaction was poured over water, extracted with EtOAc, dried over Na2SO4, evaporated in vacuo and filtered over silica gel (50% EtOAc in THF) to provide the desired amide (530 mg).

후처리

  1. customwas bubbled until saturation
  2. additionThe reaction was poured over water
  3. extractionextracted with EtOAc
  4. dry with materialdried over Na2SO4
  5. customevaporated in vacuo
  6. filtrationfiltered over silica gel (50% EtOAc in THF)

출처 및 근거

ORD 기록
ord-123036ca79af4ffc871ceb1d5ffa7a11
출처 데이터셋
uspto-grants-1997_06
특허 번호
US05639780

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