Ammonia → HCID 19041650、化合物

HRID 1684013

反応式

HRID 1684013 の反応式
[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

参加物

7

反応物 4

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

生成物 1

HCID 19041650HCID 19041650、化合物

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-123036ca79af4ffc871ceb1d5ffa7a11
出典データセット
uspto-grants-1997_06
特許番号
US05639780

関連ノート

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