Methanol → HCID 22672527、化合物

HRID 47969

反応式

HRID 47969 の反応式
[CH3:1][C:2]([CH3:26])([CH3:25])[C:3]([O:5][C:6]1[CH:7]=[CH:8][C:9]2[N:10]=[C:11]3[C:16]([O:17][C:18]=2[CH:19]=1)=[CH:15][C:14](=[O:20])[C:13]([CH2:21][CH2:22][CH2:23][OH:24])=[CH:12]3)=[O:4].C(N(CC)CC)C.[CH:34]([N:37]([CH:45]([CH3:47])[CH3:46])[P:38](Cl)[O:39][CH2:40][CH2:41][C:42]#[N:43])([CH3:36])[CH3:35].CO>C(Cl)Cl.CCOCC.CCCCCC>[CH3:1][C:2]([CH3:26])([CH3:25])[C:3]([O:5][C:6]1[CH:7]=[CH:8][C:9]2[N:10]=[C:11]3[C:16]([O:17][C:18]=2[CH:19]=1)=[CH:15][C:14](=[O:20])[C:13]([CH2:21][CH2:22][CH2:23][O:24][P:38]([N:37]([CH:45]([CH3:47])[CH3:46])[CH:34]([CH3:35])[CH3:36])[O:39][CH2:40][CH2:41][C:42]#[N:43])=[CH:12]3)=[O:4]

参加物

8

反応物 4

HCID 887MethanolHCID 8471TriethylamineHCID 27348442-Cyanoethyl N,N-diisopropylchlorophosphoramiditeHCID 226725258-(3-Hydroxypropyl)-7-oxophenoxazin-3-yl 2,2-dimethylpropanoate

生成物 1

HCID 22672527HCID 22672527、化合物

試薬・触媒・溶媒 3

HCID 3283Diethyl Ether溶媒HCID 6344Dichloromethane溶媒HCID 8058Hexane溶媒

実験手順

36b (0.38 g, 1.1 mmol) was dissolved in 6 mL of anhydrous CH2Cl2. Triethylamine (1.5 mL) was added followed by 2-cyanoethyl diisopropylchlorophosphoramidite (0.29 mL, 1.3 mmol). The solution was kept at room temperature for 30 min, MeOH (0.1 mL) was added and the reaction was concentrated under vacuum. The residue obtained was partitioned between ethyl acetate and NaHCO3. The organic phase was washed with saturated NaCl, dried over Na2SO4 and concentrated to afford the crude amidite. It was dissolved in 2 mL of ether and added dropwise to ˜50 mL of hexane. The resultant orange solid was collected by filtration, washed with hexane and dried. The yield was 0.4 g.

後処理

  1. concentrationthe reaction was concentrated under vacuum
  2. customThe residue obtained
  3. customwas partitioned between ethyl acetate and NaHCO3
  4. washThe organic phase was washed with saturated NaCl
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated
  7. customto afford the crude amidite
  8. filtrationThe resultant orange solid was collected by filtration
  9. washwashed with hexane
  10. customdried

出典と根拠

ORDレコード
ord-12f83a610c1f470193d59c21eab882af
出典データセット
uspto-grants-2004_03
特許番号
US06699975B2

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