Hydrochloric Acid → HCID 22467265, 화합물

HRID 381336노트

반응식

HRID 381336 반응식
[BH4-].[Na+].[CH:3]([C:5]1[CH:13]=[C:12]2[C:8]([C:9]([CH:15]([C:31]3[CH:39]=[C:38]([O:40][CH3:41])[C:34]4[O:35][CH2:36][O:37][C:33]=4[CH:32]=3)[C:16]([NH:18][S:19]([C:22]3[CH:27]=[CH:26][C:25]([CH3:28])=[CH:24][C:23]=3[O:29][CH3:30])(=[O:21])=[O:20])=[O:17])=[CH:10][N:11]2[CH3:14])=[CH:7][CH:6]=1)=[O:4].O.Cl>C(O)C.O1CCOCC1>[OH:4][CH2:3][C:5]1[CH:13]=[C:12]2[C:8]([C:9]([CH:15]([C:31]3[CH:39]=[C:38]([O:40][CH3:41])[C:34]4[O:35][CH2:36][O:37][C:33]=4[CH:32]=3)[C:16]([NH:18][S:19]([C:22]3[CH:27]=[CH:26][C:25]([CH3:28])=[CH:24][C:23]=3[O:29][CH3:30])(=[O:21])=[O:20])=[O:17])=[CH:10][N:11]2[CH3:14])=[CH:7][CH:6]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 4311764Sodium borohydrideHCID 22467205HCID 22467205, 화합물

생성물 1

HCID 22467265HCID 22467265, 화합물수율 79.2%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 312751,4-Dioxane용매

실험 절차

Sodium borohydride (9 mg) was added to s suspension of 6-formyl-3-{1-(7-methoxy-1,3-benzodioxol-5-yl)-2-[(2-methoxy-4-methylphenyl)sulfonamido]-2-oxoethyl}-1-methyl-1H-indole (from Example 96, 130 mg, 0.24 mmol) in a mixture of ethanol (3 ml) and 1,4-dioxane (3 ml) at ambient temperature. Stirring was continued for 1.5 hours, and then water was added dropwise until a solution was achieved. After carefully acidifying with drops of concentrated hydrochloric acid, the solvents were evaporated in vacuo. The residue was partitioned between ethyl acetate and water, and the organic layer was separated and rewashed with water. The organic layer was dried (magnesium sulphate) and the solvents removed in vacuo. The residue was crystallised from a mixture of methanol and diethyl ether to give the title compound (105 mg).

후처리

  1. customthe solvents were evaporated in vacuo
  2. customThe residue was partitioned between ethyl acetate and water
  3. customthe organic layer was separated
  4. dry with materialThe organic layer was dried (magnesium sulphate)
  5. customthe solvents removed in vacuo
  6. customThe residue was crystallised from a mixture of methanol and diethyl ether

출처 및 근거

ORD 기록
ord-55fd0dd8296d42c486fdf5fb275152b8
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06306852B1

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