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

HRID 1846439노트

반응식

HRID 1846439 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fdcbdc1e35564c5fb8ef3365c1af8bf2
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08952014B2

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