Tris(2-carboxyethyl)phosphine hydrochloride → 1,2,7-trimethyl-1H-benzimidazol-5-ylamine hydrochloride

HRID 1846439ノート

反応式

HRID 1846439 の反応式
[N:1]([C:4]1[CH:14]=[C:13]([CH3:15])[C:7]2[N:8]([CH3:12])[C:9]([CH3:11])=[N:10][C:6]=2[CH:5]=1)=[N+]=[N-].[ClH:16].C(CCP(CCC(O)=O)CCC(O)=O)(O)=O>O1CCOCC1>[ClH:16].[CH3:12][N:8]1[C:7]2[C:13]([CH3:15])=[CH:14][C:4]([NH2:1])=[CH:5][C:6]=2[N:10]=[C:9]1[CH3:11]

参加物

4

反応物 2

HCID 2734570Tris(2-carboxyethyl)phosphine hydrochlorideHCID 866638995-azido-1,2,7-trimethyl-1H-benzimidazole

生成物 1

HCID 669781471,2,7-trimethyl-1H-benzimidazol-5-ylamine hydrochloride

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

Under a nitrogen atmosphere, 200 mg (1.00 mmol) 5-azido-1,2,7-trimethyl-1H-benzimidazole, 420 mg (1.50 mmol) tris(2-carboxyethyl)phosphine-hydrochloride, 1.5 mL dioxane and 0.5 mL E-water were combined and the mixture was stirred at RT overnight. Then the reaction mixture was acidified and extracted with EtOAc. The aqueous phase was made alkaline with aqueous sodium hydroxide solution and extracted with DCM. The organic phase was dried on sodium sulphate, filtered and evaporated down. The residue was combined with ethereal hydrochloric acid and the hydrochloride that settled out as precipitate was suction filtered and dried.

後処理

  1. extractionextracted with EtOAc
  2. extractionextracted with DCM
  3. customThe organic phase was dried on sodium sulphate
  4. filtrationfiltered
  5. customevaporated down
  6. filtrationfiltered
  7. customdried

出典と根拠

ORDレコード
ord-fdcbdc1e35564c5fb8ef3365c1af8bf2
出典データセット
uspto-grants-2015_02
特許番号
US08952014B2

反応ノート

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