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Hydrochloric Acid → HCID 178481636、化合物

HRID 75637
ノート
印刷プレビュー

反応式

HRID 75637 の反応式
CNC1[N:8]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[C:7](=[O:15])[N:6]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[C:5](=[O:22])[C:4]=1[C:23]([NH:25]C(=O)OCC)=[S:24].[CH3:31][N:32]([CH3:35])[CH:33]=[O:34].C(N(CC)CC)C.Cl>O>[SH:24][C:23]1[C:4]2[C:5](=[O:22])[N:6]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[C:7](=[O:15])[N:8]([C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=3)[C:31]=2[N:32]([CH3:35])[C:33](=[O:34])[N:25]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6228DimethylformamideHCID 8471TriethylamineHCID 59717261Ethyl (6-methylamino-2,4-dioxo-1,3-diphenyl-1,2,3,4-tetrahydro-pyrimidine-5-thiocarbonyl)-carbamate

生成物 1

HCID 178481636HCID 178481636、化合物

試薬・触媒・溶媒 1

HCID 962Water
溶媒

実験手順

To crude ethyl (6-methylamino-2,4-dioxo-1,3-diphenyl-1,2,3,4-tetrahydro-pyrimidine-5-thiocarbonyl)-carbamate 23 (1.58 g) obtained in Step 4 was added N,N-dimethylformamide (8.4 ml), triethylamine (0.63 ml) was added under a nitrogen atmosphere, and the mixture was stirred at room temperature for 30 min. Water (25 ml) was added, the mixture was stirred, 1N hydrochloric acid (5.0 ml) was added, and the mixture was stirred at room temperature for 1 hr. The crystals were collected by filtration, washed with water and dried to give crude 5-mercapto-8-methyl-1,3-diphenyl-1H,8H-pyrimido[4,5-d]pyrimidine-2,4,7-trione 24 (1.53 g, over weight) as yellow crystals, which were used for the next step without purification.

後処理

  1. additionwas added under a nitrogen atmosphere
  2. stirringthe mixture was stirred
  3. stirringthe mixture was stirred at room temperature for 1 hr
  4. filtrationThe crystals were collected by filtration
  5. washwashed with water
  6. customdried

出典と根拠

ORDレコード
ord-c1e67dcd5c0e4f6bbc518c1f76dab2c6
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08835443B2

反応ノート

読み込み中…

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