Nitrogen → HCID 9864542、化合物

HRID 2268846ノート

反応式

HRID 2268846 の反応式
[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Cl:21])[C:7]=1[CH2:8][C:9]1[C:18]2[C:13](=[CH:14][C:15]([O:19][CH3:20])=[CH:16][CH:17]=2)[CH2:12][NH:11][N:10]=1.N#N.C(N(CC)CC)C.[C:31](Cl)(=[O:34])[CH2:32][CH3:33]>C1COCC1>[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Cl:21])[C:7]=1[CH2:8][C:9]1[C:18]2[C:13](=[CH:14][C:15]([O:19][CH3:20])=[CH:16][CH:17]=2)[CH2:12][N:11]([C:31](=[O:34])[CH2:32][CH3:33])[N:10]=1

参加物

6

反応物 4

HCID 947NitrogenHCID 8471TriethylamineHCID 62324Propionyl chlorideHCID 9797215Phthalazine, 4-[(3,5-dichloro-4-pyridinyl)methyl]-1,2-dihydro-7-methoxy-

生成物 1

HCID 9864542HCID 9864542、化合物収率 86%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 4-(3,5-dichloro-pyridin-4-ylmethyl)-7-methoxy-1,2-dihydro-phthalazine (1 g, 3.1 mmoles), prepared as described in example 22, in THF (35 ml), under stirring and dry N2 at room temperature, was dropwise added with triethylamine (1.08 ml, 7.76 mmoles), then, at 0° C., with propionyl chloride (0.323 ml, 3.72 mmoles). After 10 minutes the mixture was brought to room temperature and after 3 hours poured into water/ice and THF was evaporated. The mixture was extracted more times with CH2Cl2 and the organic phases were washed with 5% NaOH and water, anhydrified and brought to dryness to give a solid which was crystallised from acetonitrile (50 ml). 1 g of the title compound was obtained (yield: 86%). m.p.: 195-197° C.

後処理

  1. customat 0° C.
  2. customwas evaporated
  3. extractionThe mixture was extracted more times with CH2Cl2
  4. washthe organic phases were washed with 5% NaOH and water
  5. customto give a solid which
  6. customwas crystallised from acetonitrile (50 ml)

出典と根拠

ORDレコード
ord-6e03a02111b04981beb8abde3534c1f1
出典データセット
uspto-grants-2001_12
特許番号
US06329370B1

反応ノート

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