Ethylamine hydrochloride → HCID 16222413、化合物

HRID 237346ノート

反応式

HRID 237346 の反応式
[CH3:1][CH2:2][N:3](C(C)C)C(C)C.[CH:10]1[C:23]2[NH:22][C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[S:15][C:14]=2[CH:13]=[CH:12][C:11]=1[C:24]([OH:26])=O.Cl.C(N)C.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.C([O-])(O)=O.[Na+]>CN(C=O)C.CCOCC.CCOC(C)=O>[CH2:2]([NH:3][C:24]([C:11]1[CH:12]=[CH:13][C:14]2[S:15][C:16]3[C:21](=[CH:20][CH:19]=[CH:18][CH:17]=3)[NH:22][C:23]=2[CH:10]=1)=[O:26])[CH3:1]

参加物

9

反応物 5

HCID 11198Ethylamine hydrochlorideHCID 81531DiisopropylethylamineHCID 516892Sodium BicarbonateHCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 2271159310H-Phenothiazine-2-carboxylic acid

生成物 1

HCID 16222413HCID 16222413、化合物

試薬・触媒・溶媒 3

HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
0 °C

実験手順

5.8 ml (3.3 eq.) of DIEA is added dropwise to a solution of 2.43 g (10 mmoles) of 10H-phenothiazine-2-carboxylic acid, 1.79 g (2.2 eq.) of ethylamine hydrochloride and 4.17 g (1.1 eq.) of HBTU in 50 ml of DMF, cooled down to 0° C. The reaction mixture is stirred for 15 hours at 23° C., and then poured into a mixture of 100 ml of a saturated solution of NaHCO3 and 100 ml of AcOEt. After stirring for a few minutes, the precipitate formed is removed by filtration and the filtrate is decanted. The organic phase is successively washed with water, a 1M solution of citric acid and salt water. The organic solution is dried over sodium sulphate, filtered and concentrated to dryness under vacuum. The solid obtained is suspended in Et2O, triturated and filtered. A beige solid is obtained with a quantitative yield. Melting point: 150-151° C.

後処理

  1. stirringAfter stirring for a few minutes
  2. customthe precipitate formed
  3. customis removed by filtration
  4. customthe filtrate is decanted
  5. washThe organic phase is successively washed with water
  6. dry with materialThe organic solution is dried over sodium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated to dryness under vacuum
  9. customThe solid obtained
  10. customtriturated
  11. filtrationfiltered
  12. customA beige solid is obtained with a quantitative yield

出典と根拠

ORDレコード
ord-676ec24f2d3d4176bda46d1aed4ebd4b
出典データセット
uspto-grants-2014_02
特許番号
US08642591B2

反応ノート

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