Ammonia → HCID 59639592、化合物

HRID 556664ノート

反応式

HRID 556664 の反応式
C[Al](C)C.[NH3:5].[F:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([F:13])[C:8]=1[N:14]1[C:19]2[N:20]=[C:21]([NH:32][CH2:33][C:34](OC)=[O:35])[N:22]=[C:23]([C:24]3[CH:29]=[CH:28][C:27]([F:30])=[CH:26][C:25]=3[CH3:31])[C:18]=2[CH:17]=[CH:16][C:15]1=[O:38]>ClCCl.CCOC(C)=O>[F:13][C:9]1[CH:10]=[CH:11][CH:12]=[C:7]([F:6])[C:8]=1[N:14]1[C:19]2[N:20]=[C:21]([NH:32][CH2:33][C:34]([NH2:5])=[O:35])[N:22]=[C:23]([C:24]3[CH:29]=[CH:28][C:27]([F:30])=[CH:26][C:25]=3[CH3:31])[C:18]=2[CH:17]=[CH:16][C:15]1=[O:38]

参加物

6

反応物 3

HCID 222AmmoniaHCID 16682925TrimethylaluminumHCID 59639612HCID 59639612、化合物

生成物 1

HCID 59639592HCID 59639592、化合物収率 54%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a soln of trimethylaluminum (3.3 mL, 6.6 mmol) in dichloromethane was bubbled NH3 gas for 30 min, the product of Example 190 (500 mg, 1.1 mmol) was then added. The resulting mixture was stirred for 16 h. The mixture was diluted with EtOAc and washed with H2O to give the crude material. Purification by flash chromatography, eluting with EtOAc/triethylamine (100/2, v/v), gave the desired product (263 mg, 54%). LC-MS: 440.0 (MH+, m/z), 1.75 (Rt, min).

後処理

  1. washwashed with H2O
  2. customto give the crude material
  3. customPurification by flash chromatography
  4. washeluting with EtOAc/triethylamine (100/2

出典と根拠

ORDレコード
ord-29420105323c4c18893539239083445e
出典データセット
uspto-grants-2011_11
特許番号
US08058282B2

反応ノート

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