Diisopropylethylamine → HCID 178473956、化合物

HRID 858300ノート

反応式

HRID 858300 の反応式
[C:1]([N:4]1[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([Cl:13])[CH:11]=2)[CH2:6][C:5]1=[O:14])(=[O:3])[CH3:2].[CH3:15][N:16]1[C:20]2[CH:21]=[CH:22][C:23]([C:25](O)=[O:26])=[CH:24][C:19]=2[N:18]=[CH:17]1.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.C(N(C(C)C)C(C)C)C>CN(C=O)C.O>[C:1]([N:4]1[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([Cl:13])[CH:11]=2)[C:6](=[C:25]([OH:26])[C:23]2[CH:22]=[CH:21][C:20]3[N:16]([CH3:15])[CH:17]=[N:18][C:19]=3[CH:24]=2)[C:5]1=[O:14])(=[O:3])[CH3:2]

参加物

7

反応物 4

HCID 81531DiisopropylethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 49130631-Methyl-1H-benzimidazole-5-carboxylic acidHCID 116441611-Acetyl-6-chloroindolin-2-one

生成物 1

HCID 178473956HCID 178473956、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

3.5 g of 1-acetyl-6-chloro-2-indolinone, 3.4 g of 1-methylbenzimidazole-5-carboxylic acid, 6.1 g of TBTU, 2.9 g of HOBT-hydrate and 8.7 ml ethyldiisopropylamine are stirred in 100 ml DMF for 15 hours at ambient temperature. The mixture is combined with water and extracted with ethyl acetate, while the crude product is partially precipitated. The residue obtained by distilling off the solvent is taken up in dichloromethane and a little methanol and extracted with water. The organic phase is evaporated down, the residue stirred successively with ethyl acetate and diethyl ether, suction filtered and dried.

後処理

  1. extractionextracted with ethyl acetate, while the crude product
  2. customis partially precipitated
  3. customThe residue obtained
  4. distillationby distilling off the solvent
  5. extractiona little methanol and extracted with water
  6. customThe organic phase is evaporated down
  7. filtrationfiltered
  8. customdried

出典と根拠

ORDレコード
ord-7edb584066814722a69e407c4a7261c6
出典データセット
uspto-grants-2006_12
特許番号
US07148249B2

反応ノート

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